JP4569850B2 - Automatic synthesizer - Google Patents

Automatic synthesizer Download PDF

Info

Publication number
JP4569850B2
JP4569850B2 JP26954498A JP26954498A JP4569850B2 JP 4569850 B2 JP4569850 B2 JP 4569850B2 JP 26954498 A JP26954498 A JP 26954498A JP 26954498 A JP26954498 A JP 26954498A JP 4569850 B2 JP4569850 B2 JP 4569850B2
Authority
JP
Japan
Prior art keywords
reaction
reaction vessel
block
container
vessel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
JP26954498A
Other languages
Japanese (ja)
Other versions
JP2000093787A (en
Inventor
隆明 井上
豊 蔵谷
顕一 北村
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP26954498A priority Critical patent/JP4569850B2/en
Publication of JP2000093787A publication Critical patent/JP2000093787A/en
Application granted granted Critical
Publication of JP4569850B2 publication Critical patent/JP4569850B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00281—Individual reactor vessels
    • B01J2219/00283—Reactor vessels with top opening
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00281—Individual reactor vessels
    • B01J2219/00286—Reactor vessels with top and bottom openings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00306—Reactor vessels in a multiple arrangement
    • B01J2219/00308—Reactor vessels in a multiple arrangement interchangeably mounted in racks or blocks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00306—Reactor vessels in a multiple arrangement
    • B01J2219/00308—Reactor vessels in a multiple arrangement interchangeably mounted in racks or blocks
    • B01J2219/0031—Reactor vessels in a multiple arrangement interchangeably mounted in racks or blocks the racks or blocks being mounted in stacked arrangements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00585—Parallel processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/0059—Sequential processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00596—Solid-phase processes
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B60/00—Apparatus specially adapted for use in combinatorial chemistry or with libraries
    • C40B60/14—Apparatus specially adapted for use in combinatorial chemistry or with libraries for creating libraries

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Control Of Fluid Pressure (AREA)

Description

【０００１】
【発明の属する技術分野】
本発明は、化合物の合成を行う自動合成機に関し、特に反応容器からの内容物の漏れ防止を行う機構に関する。
【０００２】
【従来の技術】
製薬、ライフサイエンス、化学、材料等の研究分野では化合物を自動合成する自動合成機が知られている。複数の化合物の同時合成を行う自動合成機も知られており、複数の化合物を試験的に同時合成し、合成した化合物を用いて合成物の特性や合成条件等の測定を行う場合がある。
【０００３】
従来の合成器は、同時合成のために複数の反応室を備えており、個々の反応室は集合して一体となり、反応容器を形成している。この反応容器は、反応室を外部雰囲気から遮断し、かつ、ろ過ができる機能を備えている。
【０００４】
さらに、ヒータや冷却装置で温度制御された部品を押し付けることにより、反応室を所望の温度に制御できる。
【０００５】
【発明が解決しようとする課題】
従来の合成機の反応部は、複数の反応室が一つの反応容器に一体に形成された構成であるため、個々の反応室を切り離すことができず、反応室に一つでも破損や汚染が発生した場合には、反応容器全体をブロックごと交換しなければならず、反応容器にむだが発生するという問題点がある。そこで、本出願人は、反応容器と、反応容器を着脱可能とする収納部を有する反応ブロックとを備え、反応ブロックによって収納部内に収納した反応容器の反応条件の制御を行うことによって、反応容器の交換時のむだを減少させる構成を出願している（特願平９−２６６５０７号）。
上記構成において反応容器を加熱した場合、反応容器内の内容物が温度膨張あるいは気化によって反応容器から漏れ出す場合がある。通常、反応容器の排出側は生成物を排出するために大気側に開放されるのに対して、反応容器の注入側はガスの注入等のために反応時には密閉状態としている。そのため、反応容器から膨出した内容物は排出側に漏れ出すことになる。
【０００６】
図１０は内容物の漏出を説明するための図である。図１０において、合成機は反応ブロック５と排出容器８とを備え、反応容器３は反応ブロック５の収納部内に収納される。反応容器３は反応室３１を備える。反応室３１内の内容物が温度膨張したり気化すると、内容物は導出管３２を通って排出容器８内の空間９に漏出される。内容物が粘性が高い液体である場合には、いったん漏出が始まると反応室３１から内容物が排出し終わるまで漏出が続くことになる。
【０００７】
そこで、本発明は前記した問題点を解決し、反応容器内の内容物の排出を制御することを目的とし、特に反応室からの内容物の漏出を防止することを目的とする。
【０００８】
【課題を解決するための手段】
本発明の自動合成機は、反応ブロックの排出側の圧力を調整することによって、反応容器内外の圧力差を調整し、これによって反応容器内の内容物の排出の制御を行う。特に、反応ブロックの排出側の圧力を高めて、反応容器の外側の圧力を反応容器内部の圧力より高めることによって、反応容器からの容物の漏出を防止するものである。
【０００９】
本発明は、化学反応により化合物を合成する自動合成機において、反応容器を着脱可能とする収納部を有する反応ブロックと、反応容器内の内容物を排出する排出容器と、反応ブロックと排出容器とで形成される密閉空間内の圧力を調整する圧力調整手段を備え、前記反応容器は、一端を当該反応容器内に通し、他端を前記底部よりも下方位置で排出容器側に開放し、前記両端部分の間に両端の位置よりも高い部分を有し、当該反応容器の内部と外部とを連通する導出管を備え、圧力調整手段は、ガス供給源から密閉空間内にガスを導入して加圧して圧力を高め、この加圧によって反応容器からの内容物の排出を抑制する。
【００１０】
反応ブロックと排出容器とを密着させて接合させることにより、排出容器内部は反応ブロックで密閉され密閉空間が形成される。圧力調整手段は、密閉空間内の圧力を調整することによって反応容器内外に圧力差を形成し、反応容器内の内容物の排出制御を行う。反応容器内より反応容器外の圧力を高めた場合には、反応容器内から内容物が流れでることを防止することができる。また、反応容器内より反応容器外の圧力を低めた場合には、反応容器内からの内容物の排出を促進することができる。
【００１１】
本発明の圧力調整手段として加圧手段を適用した形態をとることができる。加圧手段により反応容器内を加圧することによって反応容器内の内容物の排出制御を行う構成とし、これによって、反応室からの内容物の漏出を防止することができる。なお、このとき反応容器の注入側は上蓋やシール材等によって密閉状態にあり、反応容器内の内容物が注入側から漏出することはない。
【００１２】
加圧手段の実施の一形態は反応容器内へのガス供給による形態とすることができる。密閉空間内にガスを供給することによって内部圧力を高め、該密閉空間と連通する反応ブロックの排出側及び反応容器の排出側の圧力を反応容器の内部の圧力より高くする。この圧力差によって、反応容器内の内容物が排出容器側に漏出することを防止する。
【００１３】
本発明のガス供給による加圧手段の第１の形態は、排出容器の空間内にガスを供給する流路を反応ブロック側に備えるものである。ガス供給源から該流路を通して排出容器の空間内にガスを導入し、導入したガスによって排出容器内の圧力を高める。
【００１４】
図１，２は第１の形態の加圧手段を備える自動合成機の一構成を説明するための斜視図及び断面図である。図１，２において、自動合成機１は反応ブロック５と排出容器８とを備え、反応容器３は反応ブロック５の収納部内に収納される。反応容器３を収納した後、反応ブロック５は上蓋７，及びシール材６によって密閉される。
【００１５】
反応ブロック５と排出容器８とを密着させて接合させることによって、排出容器８内の空間９は密閉された空間となる。反応ブロック５は外部と排出容器８内の空間９とを連通する流路１０を備える。外部に設けた図示しないガス供給源から流路１０を通してガスを排出容器８の空間９内に導入する。空間９は密閉状態にあるため、ガス導入によって内部の圧力は反応容器３側の圧力より高まり、反応容器３内の内容物が導出管３２を通して排出容器８側に漏出することを防止する。なお、このとき反応容器３の注入側は上蓋７，及びシール材６等によって密閉状態にあり、反応容器３内の内容物が注入側から漏出することはない。
【００１６】
本発明のガス供給による加圧手段の第２の形態は、排出容器の空間内にガスを供給する流路を排出容器側に備えるものである。加圧手段の第１の形態と同様に、ガス供給源から流路を通して排出容器の空間内にガスを導入し、導入したガスによって排出容器内の圧力を高める。
【００１７】
図３は第２の形態の加圧手段を備える自動合成機の一構成を説明するための斜視図である。図３において、自動合成機１は、流路の構成を除いて図１の構成とほぼ同様の構成を備える。流路１０は排出容器９側に形成され、該流路１０を通して外部と排出容器８内の空間９とを連通し、外部に設けた図示しないガス供給源から流路１０を通してガスを排出容器８の空間９内に導入する。排出容器８内に導入したガスは、第１の形態と同様の作用によって反応容器３内の内容物が導出管３２を通して排出容器８側に漏出することを防止する。
【００２２】
前記各形態において、供給するガスは反応容器での化学反応に影響を与えないガス種とし、一般的には不活性ガスである窒素ガスやアルゴンガスを用いることができる。
本発明の加圧手段を用いた実施の態様によれば、反応容器内の内容物の排出を制御することができ、特に反応室からの内容物の漏出を防止することができる。
【００２３】
また、本発明の加圧手段を用いた実施の態様によれば、反応ブロックあるいは排出容器を流路とする構成であるため、自動合成機の他の機構の動作に影響を与えることなく内容物の漏出防止を行うことができる。
【００２４】
【発明の実施の形態】
以下、本発明の実施の形態を図を参照しながら詳細に説明する。図４は本発明の自動合成機の概略を説明するための一部を切り欠いた斜視図であり、加圧手段の第１，２の形態を示している。なお、以下で説明する各実施の形態では、反応ブロックと共に還流ブロックを備えた構成例について説明する。
【００２５】
図４において、本発明の自動合成機１は反応容器３及び還流容器２を複数個備え、各反応容器３内に試薬や溶媒等の合成に必要な物質を注入し、温度，圧力，振とう，周囲雰囲気等の条件制御下で反応及びろ過を行い、化合物の合成を行う。反応容器３は、合成に必要な物質を注入し化合物の合成を行う反応室３１と、フィルターでろ過したろ過物質を外部に取り出す導出管３２と、導出管３２等の細管のつまりを除くための保守用押しねじを備える（図２参照）。又、還流容器２は、反応容器３内で気化した物質を凝縮させて液化させるための容器であって、反応容器３の上方に取り付けられ、反応容器３内への物質の注入を行うための開口部と、気密性を保持するためのＯリング等のパッキングを備える。なお、反応容器３及び還流容器２はテフロン（登録商標），ポリプロピレン等の合成樹脂で形成することができる。テフロンを用いた場合には化学反応に対する耐性が良く、ポリプロピレンを用いた場合には安価で形成することができ、使い捨てが容易となる。
【００２６】
自動合成機反応部１は還流ブロック４と反応ブロック５を備える。還流ブロック４は、アルミニウム等で形成される伝熱部材を兼ねた還流ブロック本体４１と、還流ブロック本体４１の下面に取り付けられて、熱媒流路４８を保持する熱媒流路押さえ４２とを有している。熱媒流路押さえ４２は断熱材を兼ねることができ、テフロンで形成することができる。
【００２７】
還流ブロック本体４１には複数個の還流容器２を収納する複数の収納部４３が形成され、上面には反応容器３内に試薬や溶媒等の合成に必要な物質を注入するための開口部が形成され、又、熱媒流路押さえ４２には還流容器２のフランジ部分やパッキングを収納する凹部が形成される。又、還流ブロック本体４１内には、熱媒流路４８を収納部４３と交差しないよう配置する。熱媒流路４８中に熱媒を流すことによって、還流ブロック本体４１を伝熱部材として、収納部４３内に収納した還流容器２の温度制御を行う。例えば、熱媒の温度が０℃であれば、熱媒流路４８と接触している還流ブロック本体４１を介して還流容器２も熱媒に近い温度に冷却される。
【００２８】
還流ブロック本体４１に対する還流容器２の脱着は、熱媒流路押さえ４２に形成された開口部を通して行い、還流容器２のフランジ部を還流ブロック本体４１及び熱媒流路押さえ４２ではさみ、図示しない固定具で固定することによって還流容器２の所定位置への固定を行うことができる。
【００２９】
還流ブロック４の上面には、テフロン、フッ素ゴム等で形成されるシール材６をはさんでアルミニウム等で形成される上蓋７が取り付けられる。還流ブロック４の上面とシール材６との間の密着性を高めて外気との遮断を行うために、還流ブロック４の上面に溝４５を形成し、該溝４５内にシール材６に形成した凸部６１を押し込む構成とすることができる。
【００３０】
又、還流ブロック４の上面の収納部４３に隣接してガス用溝４４を形成し、このガス用溝４４を通して反応容器３内に窒素やアルゴン等の不活性ガスを供給し、その圧力によってフィルターを通してろ過させ、反応容器３内の液体成分の排出を行うことができる。なお、上記ガス用溝４４に代えて、シール材６に円筒形のニードルを突き刺し、不活性ガスを供給する構成とすることもできる。この構成によれば、反応容器の内容物を個別にろ過することができる。
【００３１】
又、上蓋７には、還流容器２及び反応容器３に通じる開口部７１が形成され、該開口部７１を通して上記ニードル等をシール材６に貫通させ、反応容器３内に試薬や溶媒等の合成に必要な物質の注入や不活性ガスの供給を行うことができる。
【００３２】
反応ブロック５は、アルミニウム等で形成される伝熱部材を兼ねた反応ブロック本体５１と、反応ブロック本体５１の上面に取り付けられて、熱媒流路５８を保持する熱媒流路押さえ５４と、反応ブロック本体５１の下面に取り付けられて、ヒータ５９を保持するヒータ押さえ５２とを有している。両押さえ５２，５４は断熱材を兼ねることができ、テフロンで形成することができる。
【００３３】
反応ブロック本体５１には複数個の反応容器３を収納する複数の収納部５３が形成され、熱媒流路押さえ５４には反応容器３を挿入し、上端部分を突出させるための開口部が形成され、ヒータ押さえ５２には反応容器３の導出部３２を外部に通すための開口部５５が形成される。反応ブロック本体５１に対する反応容器３の脱着は、熱媒流路押さえ５４に形成された開口部を通して行い、反応容器３の底部をヒータ押さえ５２に当接させることによって反応容器３の位置決めを行うことができる。
【００３４】
又、反応ブロック本体５１内には、熱媒流路５８及びヒータ５９が配置される。熱媒流路５８中に熱媒を流すことによって、反応ブロック本体５１を伝熱部材として収納部５３内に収納した反応容器３を冷却または加熱する。又、ヒータ５９を駆動することによって、反応ブロック本体５１を伝熱部材として収納部５３内に収納した反応容器３を加熱する。
【００３５】
例えば、熱媒の温度が６０℃であれば、熱媒流路５８と接触している反応ブロック本体５１を介して反応容器３も熱媒に近い温度に加熱される。また、ヒータ５９によってさらに高温に加熱することができ、温度制御は図示しない温度センサとコントローラにより行うことができ、定温に保持することもできる。
【００３６】
本発明の自動合成機の反応部は、反応容器を着脱自在とする反応ブロックのみを備え、還流ブロックを省いた構成とすることもできる。
【００３７】
排出容器８は、反応ブロック５の下方に取り付けられる。図６では排出容器８の底面のみを示している。排出容器８は上方の縁部分（図示していない）を反応ブロック５（図６ではヒータ押さえ５２）に当接させて密着させて取り付ける。これによって、排出容器８の空間９は密閉された空間となる。空間９は、通常反応容器３から取り出された内容物を受ける受け部分となる。
【００３８】
本発明の自動合成機は、内容物の漏出を防止する圧力調整手段として加圧手段を備える。
加圧手段の第１の形態は、反応ブロック５側に流路１０を形成する。流路１０は自動合成機１の外部と排出容器８内の空間９とを連通する。流路１０の一端は外部に設けられた加圧手段等の圧力調整手段に接続され、排出容器８内の空間９の圧力を調整する。ガス供給による加圧手段を用いた場合、流路１０を介して空間９内にガスを供給し、空間９の圧力を高める。
【００３９】
反応容器３を加熱した場合、反応容器３内の内容物が温度膨張あるいは気化によって反応容器３内の圧力が高まり、内容物が排出容器８の空間９に漏れ出そうとする。このとき、流路１０を通して空間９内にガスを供給し、空間９内の圧力を反応容器３内の圧力より高める。この圧力差によって、反応容器３内の内容物の空間９への漏出を抑えることができる。
【００４０】
加圧手段の第２の形態は排出容器８側に流路１０を形成するものであり、第１の形態と流路の形成箇所のみ異なり他の構成は共通とすることができる。流路１０は自動合成機１の外部と排出容器８内の空間９とを連通し、第１の形態と同様の作用によって反応容器３内の内容物の空間９への漏出を抑えることができる。なお、第２の形態の詳細は第１の形態と同様であるため省略する。
【００４１】
加圧手段の第１，２の形態において、流路１０はチューブ材あるいは反応ブロックや排出容器に形成した貫通孔により形成することができる。
【００４９】
次に、本発明の自動合成機による合成手順について説明する。収納部５３内に反応容器３を収納した反応ブロック５１と、収納部４３内に還流容器３を収納した還流ブロック４１を用意し、反応ブロック５１の熱媒流路押さえ５４に上面に還流ブロック４を取り付け、さらに、還流ブロック４１の上面にシール材６及び上蓋７を取り付け、固定具で固定を行うことにより自動合成機反応部１の組立を行う。
【００５０】
この組立において、反応容器３内に反応に用いる試薬や溶媒の注入を行う。なお、自動合成機反応部１の組立の後、上蓋７に形成した開口部７１を通してシール材６にニードルを刺し込み、反応容器３内に反応に用いる試薬や溶媒の注入を行うこともできる。
【００５１】
反応ブロック３の熱媒流路５８に熱媒を流したり、ヒータ５９を駆動することによって、反応容器３内の試薬や溶媒を冷却または加熱して、反応条件の温度制御を行う。また、ガス用溝４４から不活性ガスを供給して圧力制御を行ったり、反応ブロック３全体を振とうさせることもできる。
【００５２】
加熱による反応を行わせるとき、溶媒の沸点が試薬の沸点よりも低い場合には、溶媒成分は試薬より先に気化する。気化した溶媒成分は、反応容器３の上方に設置された還流容器２に到達する。このとき、還流ブロック４中の熱媒流路４８に冷媒を流して還流容器２を冷却すると、気化した溶媒成分は冷却されて凝縮し、液体となって反応容器３内に戻される。これによって、溶媒が蒸発して消失することを防止することができる。
【００５３】
この加熱において、反応容器３内の内容物が膨張したり気化するおそれがある場合には、本発明の圧力調節手段の加圧手段によって排出容器８の空間９内の圧力を高め、反応容器３内の内容物の漏出を防ぐ。
【００５４】
反応の後、合成された物質をろ過する場合には、図示しないガス源から不活性ガスを導入し、ガス用溝４４を通して反応容器３内に流通させる。反応容器３の内部は不活性な雰囲気に保たれたまま加圧され、複数の反応容器３内の液体成分をフィルター３５を通して同時に取り出すことができる。化合物は、ろ過物あるいは、ろ過残留物として取り出すことができる。
【００５５】
また、反応容器３から生成物の取り出しは、本発明の圧力調整手段によって排出容器８の空間９内の圧力を反応容器３内の圧力より減圧することによって行うこともできる。
【００５６】
反応容器３の導出管３２の細管に穴づまりが発生した場合には、保守用押しねじ３４を外し、細い棒で導出管３２内を清掃することにより穴づまりを解消することができる。
【００５７】
又、反応容器３や還流容器２の洗浄を行う場合には、図示しない固定具を解除して還流ブロック４と反応ブロック５を分離し、還流ブロック４から還流容器２を取り外し、反応ブロック５から反応容器３を取り外して、各還流容器２及び反応容器３を洗浄することができる。また、還流ブロック４および反応ブロック５自体の洗浄を行うこともできる。洗浄した後、再び還流ブロック４内に還流容器２を挿入し、反応ブロック５内に反応容器３を挿入することによって、自動合成機の反応部を組み立てることができる。
【００５８】
前記洗浄と同様の手順によって、破損あるいは汚染された還流容器あるいは反応容器のみを正常な容器に交換することができる。本発明の圧力調整手段は、反応ブロックあるいは排出容器を流路とする構成であり、自動合成機の他の構成部分と干渉を起こさない構成であるため、他の構成部分に影響することなく洗浄や交換を行うことができる。
【００５９】
なお、反応ブロックにおける流路の形成位置、排出容器における流路の形成位置は任意とすることができる。
【００６０】
【発明の効果】
以上説明したように、本発明の自動合成機によれば、反応容器内の内容物の排出の防止、及び排出の促進等の排出制御を行うことができ、特に加熱による反応室内の内容物の膨張や気化による漏出を防止することができる。
【図面の簡単な説明】
【図１】第１の形態の加圧手段を備える自動合成機の一構成を説明するための斜視図である。
【図２】第１の形態の加圧手段を備える自動合成機の一構成を説明するための断面図である。
【図３】第２の形態の加圧手段を備える自動合成機の一構成を説明するための斜視図である。
【図４】本発明の自動合成機の概略を説明するための一部を切り欠いた斜視図である。
【図５】内容物の漏出を説明するための図である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an automatic synthesizer for synthesizing compounds, and more particularly to a mechanism for preventing leakage of contents from a reaction vessel.
[0002]
[Prior art]
In research fields such as pharmaceutical, life science, chemistry, and materials, automatic synthesizers that automatically synthesize compounds are known. An automatic synthesizer that simultaneously synthesizes a plurality of compounds is also known. In some cases, a plurality of compounds are simultaneously synthesized on a trial basis, and the synthesized compound is used to measure characteristics of the synthesized product, synthesis conditions, or the like.
[0003]
A conventional synthesizer is provided with a plurality of reaction chambers for simultaneous synthesis, and the individual reaction chambers are gathered together to form a reaction vessel. This reaction vessel has a function of blocking the reaction chamber from the external atmosphere and allowing filtration.
[0004]
Furthermore, the reaction chamber can be controlled to a desired temperature by pressing a part whose temperature is controlled by a heater or a cooling device.
[0005]
[Problems to be solved by the invention]
Since the reaction section of a conventional synthesizer has a structure in which a plurality of reaction chambers are integrally formed in one reaction vessel, individual reaction chambers cannot be separated, and even one reaction chamber is damaged or contaminated. When this occurs, the entire reaction vessel must be replaced with the entire block, causing a problem that the reaction vessel is wasteful. Therefore, the present applicant comprises a reaction vessel and a reaction block having a storage unit that allows the reaction vessel to be attached and detached, and by controlling the reaction conditions of the reaction vessel stored in the storage unit by the reaction block, the reaction vessel Has been filed for a configuration that reduces waste during replacement (Japanese Patent Application No. 9-266507).
When the reaction vessel is heated in the above configuration, the contents in the reaction vessel may leak from the reaction vessel due to temperature expansion or vaporization. Normally, the discharge side of the reaction vessel is opened to the atmosphere side to discharge the product, whereas the injection side of the reaction vessel is sealed during the reaction for gas injection or the like. Therefore, the contents swelled from the reaction vessel leaks to the discharge side.
[0006]
FIG. 10 is a view for explaining leakage of contents. In FIG. 10, the synthesizer includes a reaction block 5 and a discharge container 8, and the reaction container 3 is stored in a storage unit of the reaction block 5. The reaction vessel 3 includes a reaction chamber 31. When the content in the reaction chamber 31 expands or vaporizes, the content leaks through the outlet pipe 32 into the space 9 in the discharge container 8. When the content is a highly viscous liquid, once the leakage starts, the leakage continues until the content is completely discharged from the reaction chamber 31.
[0007]
Therefore, the present invention aims to solve the above-mentioned problems and to control the discharge of the contents in the reaction vessel, and in particular to prevent the leakage of the contents from the reaction chamber.
[0008]
[Means for Solving the Problems]
The automatic synthesizer of the present invention adjusts the pressure difference inside and outside the reaction vessel by adjusting the pressure on the discharge side of the reaction block, thereby controlling the discharge of the contents in the reaction vessel. In particular, the pressure on the discharge side of the reaction block is increased so that the pressure outside the reaction vessel is higher than the pressure inside the reaction vessel, thereby preventing leakage of contents from the reaction vessel.
[0009]
The present invention relates to an automatic synthesizer that synthesizes a compound by a chemical reaction, a reaction block having a storage section that allows the reaction container to be detachable, a discharge container that discharges the contents in the reaction container, a reaction block, and a discharge container. Pressure adjusting means for adjusting the pressure in the sealed space formed by the above, the reaction vessel, one end passes through the reaction vessel, the other end is opened to the discharge vessel side at a position below the bottom, It has a part higher than the position of both ends between both end parts, and has a lead-out pipe that communicates the inside and outside of the reaction vessel, and the pressure adjusting means introduces gas into the sealed space from the gas supply source. pressurized enhance pressure, suppressing the discharge of contents from Hence the reaction vessel to the pressure.
[0010]
By bringing the reaction block and the discharge container into close contact with each other, the inside of the discharge container is sealed with the reaction block to form a sealed space. The pressure adjusting means forms a pressure difference inside and outside the reaction container by adjusting the pressure in the sealed space, and controls the discharge of the contents in the reaction container. When the pressure outside the reaction vessel is increased from the inside of the reaction vessel, the contents can be prevented from flowing out of the reaction vessel. Further, when the pressure outside the reaction vessel is lowered from the inside of the reaction vessel, the discharge of the contents from the reaction vessel can be promoted.
[0011]
The form which applied the pressurization means as a pressure adjustment means of this invention can be taken. By controlling the discharge of the contents in the reaction container by pressurizing the inside of the reaction container by the pressurizing means, leakage of the contents from the reaction chamber can be prevented. At this time, the injection side of the reaction vessel is sealed with an upper lid, a sealing material, etc., and the contents in the reaction vessel will not leak from the injection side.
[0012]
One embodiment of the pressurizing means may be a form by supplying gas into the reaction vessel. By supplying gas into the sealed space, the internal pressure is increased, and the pressure on the discharge side of the reaction block and the discharge side of the reaction vessel communicating with the sealed space is made higher than the pressure inside the reaction vessel. This pressure difference prevents the contents in the reaction vessel from leaking to the discharge vessel side.
[0013]
The first form of the pressurizing means by gas supply of the present invention is provided with a flow path for supplying gas into the space of the discharge container on the reaction block side. A gas is introduced from the gas supply source into the space of the discharge container through the flow path, and the pressure in the discharge container is increased by the introduced gas.
[0014]
1 and 2 are a perspective view and a cross-sectional view for explaining a configuration of an automatic synthesizer including a pressurizing unit according to the first embodiment. 1 and 2, the automatic synthesizer 1 includes a reaction block 5 and a discharge container 8, and the reaction container 3 is stored in a storage unit of the reaction block 5. After housing the reaction vessel 3, the reaction block 5 is sealed with an upper lid 7 and a sealing material 6.
[0015]
By bringing the reaction block 5 and the discharge container 8 into close contact with each other, the space 9 in the discharge container 8 becomes a sealed space. The reaction block 5 includes a flow path 10 that communicates the outside with the space 9 in the discharge container 8. Gas is introduced into the space 9 of the discharge container 8 through a flow path 10 from a gas supply source (not shown) provided outside. Since the space 9 is in a hermetically sealed state, the internal pressure becomes higher than the pressure on the reaction vessel 3 side by gas introduction, and the contents in the reaction vessel 3 are prevented from leaking to the discharge vessel 8 side through the outlet tube 32. At this time, the injection side of the reaction vessel 3 is hermetically sealed by the upper lid 7 and the sealing material 6 and the contents in the reaction vessel 3 are not leaked from the injection side.
[0016]
The second form of the pressurizing means by gas supply of the present invention is provided with a flow path for supplying gas into the space of the discharge container on the discharge container side. Similar to the first embodiment of the pressurizing means, gas is introduced into the space of the discharge container from the gas supply source through the flow path, and the pressure in the discharge container is increased by the introduced gas.
[0017]
FIG. 3 is a perspective view for explaining one configuration of the automatic synthesizer including the pressurizing means of the second embodiment. In FIG. 3, the automatic synthesizer 1 has substantially the same configuration as that of FIG. 1 except for the configuration of the flow path. The flow path 10 is formed on the discharge container 9 side, communicates the outside and the space 9 in the discharge container 8 through the flow path 10, and discharges gas from the gas supply source (not shown) provided outside through the flow path 10. It is introduced into the space 9. The gas introduced into the discharge container 8 prevents the contents in the reaction container 3 from leaking to the discharge container 8 side through the outlet tube 32 by the same action as in the first embodiment.
[0022]
In each of the above embodiments, the gas to be supplied is a gas species that does not affect the chemical reaction in the reaction vessel, and generally an inert gas such as nitrogen gas or argon gas can be used.
According to the embodiment using the pressurizing means of the present invention, the discharge of the contents in the reaction vessel can be controlled, and in particular, the leakage of the contents from the reaction chamber can be prevented.
[0023]
In addition, according to the embodiment using the pressurizing means of the present invention, since the reaction block or the discharge container is used as the flow path, the contents can be obtained without affecting the operation of other mechanisms of the automatic synthesizer. Can be prevented.
[0024]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. Figure 4 is a perspective view partially cut away for illustrating an outline of an automatic synthesizer of the present invention, showing the first and second embodiment of the pressure means. In each embodiment described below, a configuration example including a reflux block together with a reaction block will be described.
[0025]
In FIG. 4 , the automatic synthesizer 1 of the present invention includes a plurality of reaction vessels 3 and reflux vessels 2, and injects substances necessary for the synthesis of reagents, solvents and the like into each reaction vessel 3, and the temperature, pressure, and shaking. The compound is synthesized by reaction and filtration under controlled conditions such as ambient atmosphere. The reaction vessel 3 is for removing the clogging of narrow tubes such as the reaction chamber 31 for injecting substances necessary for synthesis and synthesizing the compound, the outlet pipe 32 for taking out the filtered substance filtered by the filter, and the outlet pipe 32. A maintenance push screw is provided (see FIG. 2 ). The reflux vessel 2 is a vessel for condensing and liquefying the material vaporized in the reaction vessel 3, and is attached above the reaction vessel 3 for injecting the material into the reaction vessel 3. An opening and a packing such as an O-ring for maintaining airtightness are provided. The reaction vessel 3 and the reflux vessel 2 can be formed of a synthetic resin such as Teflon (registered trademark) or polypropylene. When Teflon is used, it has good resistance to chemical reaction, and when polypropylene is used, it can be formed at low cost and is easy to be disposable.
[0026]
The automatic synthesizer reaction unit 1 includes a reflux block 4 and a reaction block 5. The reflux block 4 includes a reflux block main body 41 that also serves as a heat transfer member formed of aluminum or the like, and a heat medium flow path holder 42 that is attached to the lower surface of the reflux block main body 41 and holds the heat medium flow path 48. Have. The heat medium flow path retainer 42 can also serve as a heat insulating material, and can be formed of Teflon.
[0027]
The reflux block main body 41 is formed with a plurality of storage portions 43 for storing a plurality of reflux containers 2, and an opening for injecting a substance necessary for synthesis of a reagent, a solvent, or the like into the reaction container 3 on the upper surface. In addition, the heat medium passage presser 42 is formed with a flange portion of the reflux vessel 2 and a recess for storing the packing. Further, in the reflux block main body 41, the heat medium flow path 48 is arranged so as not to intersect the storage portion 43. By flowing the heat medium in the heat medium flow path 48, the temperature of the reflux container 2 stored in the storage unit 43 is controlled using the reflux block body 41 as a heat transfer member. For example, if the temperature of the heat medium is 0 ° C., the reflux container 2 is also cooled to a temperature close to that of the heat medium via the reflux block body 41 that is in contact with the heat medium flow path 48.
[0028]
The reflux container 2 is attached to and detached from the reflux block main body 41 through an opening formed in the heat medium flow path holder 42. The flange portion of the reflux container 2 is sandwiched between the reflux block main body 41 and the heat medium flow path retainer 42 and is not shown. The reflux container 2 can be fixed at a predetermined position by fixing with a fixing tool.
[0029]
An upper lid 7 made of aluminum or the like is attached to the upper surface of the reflux block 4 with a sealing material 6 made of Teflon or fluororubber or the like interposed therebetween. In order to improve the adhesion between the upper surface of the reflux block 4 and the sealing material 6 and to block the outside air, a groove 45 is formed on the upper surface of the reflux block 4, and the sealing material 6 is formed in the groove 45. It can be set as the structure which pushes in the convex part 61. FIG.
[0030]
Further, a gas groove 44 is formed adjacent to the storage portion 43 on the upper surface of the reflux block 4, and an inert gas such as nitrogen or argon is supplied into the reaction vessel 3 through the gas groove 44. The liquid component in the reaction vessel 3 can be discharged. In place of the gas groove 44, a cylindrical needle may be inserted into the sealing material 6 to supply an inert gas. According to this configuration, the contents of the reaction vessel can be individually filtered.
[0031]
In addition, the upper lid 7 is formed with an opening 71 communicating with the reflux vessel 2 and the reaction vessel 3. Through the opening 71, the needle or the like is passed through the sealing material 6 to synthesize a reagent or a solvent in the reaction vessel 3. It is possible to inject necessary substances and supply inert gas.
[0032]
The reaction block 5 includes a reaction block main body 51 that also serves as a heat transfer member formed of aluminum or the like, a heat medium flow path retainer 54 that is attached to the upper surface of the reaction block main body 51 and holds the heat medium flow path 58, The heater block 52 is attached to the lower surface of the reaction block main body 51 and holds the heater 59. Both the pressers 52 and 54 can also serve as a heat insulating material, and can be formed of Teflon.
[0033]
The reaction block body 51 is formed with a plurality of storage portions 53 for storing a plurality of reaction vessels 3, and the heat medium flow path retainer 54 is formed with an opening for inserting the reaction vessel 3 and projecting the upper end portion. The heater holder 52 is formed with an opening 55 for allowing the lead-out portion 32 of the reaction vessel 3 to pass outside. The reaction container 3 is attached to and detached from the reaction block main body 51 through an opening formed in the heat medium flow path retainer 54, and the reaction container 3 is positioned by bringing the bottom of the reaction container 3 into contact with the heater retainer 52. Can do.
[0034]
A heat medium flow path 58 and a heater 59 are disposed in the reaction block main body 51. By flowing a heat medium through the heat medium flow path 58, the reaction vessel 3 housed in the housing part 53 using the reaction block main body 51 as a heat transfer member is cooled or heated. In addition, by driving the heater 59, the reaction vessel 3 housed in the housing portion 53 using the reaction block main body 51 as a heat transfer member is heated.
[0035]
For example, if the temperature of the heat medium is 60 ° C., the reaction vessel 3 is also heated to a temperature close to that of the heat medium through the reaction block body 51 that is in contact with the heat medium flow path 58. Further, it can be heated to a higher temperature by the heater 59, temperature control can be performed by a temperature sensor and a controller (not shown), and the temperature can be kept constant.
[0036]
The reaction unit of the automatic synthesizer of the present invention can be configured to include only a reaction block that allows the reaction vessel to be detachable, and omit the reflux block.
[0037]
The discharge container 8 is attached below the reaction block 5. FIG. 6 shows only the bottom surface of the discharge container 8. The discharge container 8 is attached by bringing the upper edge (not shown) into contact with the reaction block 5 (heater presser 52 in FIG. 6). Thereby, the space 9 of the discharge container 8 becomes a sealed space. The space 9 is a receiving portion for receiving the contents normally taken out from the reaction vessel 3.
[0038]
The automatic synthesizer of the present invention includes a pressurizing means as a pressure adjusting means for preventing leakage of contents.
In the first form of the pressurizing means, the flow path 10 is formed on the reaction block 5 side. The flow path 10 communicates the outside of the automatic synthesizer 1 and the space 9 in the discharge container 8. One end of the flow path 10 is connected to a pressure adjusting means such as a pressurizing means provided outside to adjust the pressure in the space 9 in the discharge container 8. When a pressurizing means by gas supply is used, gas is supplied into the space 9 through the flow path 10 to increase the pressure in the space 9.
[0039]
When the reaction vessel 3 is heated, the pressure in the reaction vessel 3 increases due to temperature expansion or vaporization of the content in the reaction vessel 3, and the content tends to leak into the space 9 of the discharge vessel 8. At this time, gas is supplied into the space 9 through the flow path 10, and the pressure in the space 9 is made higher than the pressure in the reaction vessel 3. Due to this pressure difference, leakage of the contents in the reaction vessel 3 into the space 9 can be suppressed.
[0040]
The second form of the pressurizing means is to form the flow path 10 on the discharge container 8 side, and is different from the first form only in the location where the flow path is formed, and other configurations can be made common. The flow path 10 communicates the outside of the automatic synthesizer 1 and the space 9 in the discharge container 8, and can suppress leakage of the contents in the reaction container 3 to the space 9 by the same action as in the first embodiment. . Note that the details of the second embodiment are the same as those of the first embodiment, and are therefore omitted.
[0041]
In the first and second forms of the pressurizing means, the flow path 10 can be formed by a tube material or a through hole formed in a reaction block or a discharge container.
[0049]
Next, a synthesis procedure by the automatic synthesizer of the present invention will be described. A reaction block 51 in which the reaction vessel 3 is housed in the housing portion 53 and a reflux block 41 in which the reflux vessel 3 is housed in the housing portion 43 are prepared. In addition, the automatic synthesizer reaction unit 1 is assembled by attaching the sealing material 6 and the upper lid 7 to the upper surface of the reflux block 41 and fixing with a fixture.
[0050]
In this assembly, reagents and solvents used for the reaction are injected into the reaction vessel 3. In addition, after the assembly of the automatic synthesizer reaction unit 1, a needle or the like can be inserted into the sealing material 6 through the opening 71 formed in the upper lid 7 to inject the reagent or solvent used for the reaction into the reaction vessel 3.
[0051]
By flowing a heat medium through the heat medium flow path 58 of the reaction block 3 or by driving a heater 59, the reagent or solvent in the reaction vessel 3 is cooled or heated to control the temperature of the reaction conditions. Further, an inert gas can be supplied from the gas groove 44 to perform pressure control, or the entire reaction block 3 can be shaken.
[0052]
When the reaction by heating is performed, if the boiling point of the solvent is lower than the boiling point of the reagent, the solvent component is vaporized before the reagent. The evaporated solvent component reaches the reflux container 2 installed above the reaction container 3. At this time, when the refrigerant is allowed to flow through the heat medium flow path 48 in the reflux block 4 to cool the reflux container 2, the evaporated solvent component is cooled and condensed, and is returned to the reaction container 3 as a liquid. This can prevent the solvent from evaporating and disappearing.
[0053]
In this heating, when the contents in the reaction vessel 3 may expand or vaporize, the pressure in the space 9 of the discharge vessel 8 is increased by the pressurizing means of the pressure adjusting means of the present invention, and the reaction vessel 3 Prevent leakage of contents inside.
[0054]
When the synthesized substance is filtered after the reaction, an inert gas is introduced from a gas source (not shown) and is circulated into the reaction vessel 3 through the gas groove 44. The inside of the reaction vessel 3 is pressurized while being maintained in an inert atmosphere, and the liquid components in the plurality of reaction vessels 3 can be simultaneously taken out through the filter 35. The compound can be taken out as a filtrate or a filtration residue.
[0055]
Further, the product can be taken out from the reaction vessel 3 by reducing the pressure in the space 9 of the discharge vessel 8 from the pressure in the reaction vessel 3 by the pressure adjusting means of the present invention.
[0056]
When clogging occurs in the narrow tube of the outlet tube 32 of the reaction vessel 3, the clogged hole can be eliminated by removing the maintenance push screw 34 and cleaning the inside of the outlet tube 32 with a thin rod.
[0057]
Further, when washing the reaction vessel 3 and the reflux vessel 2, a fixing tool (not shown) is released to separate the reflux block 4 and the reaction block 5, and the reflux vessel 2 is detached from the reflux block 4 and the reaction block 5 is removed. The reaction vessel 3 can be removed and each reflux vessel 2 and the reaction vessel 3 can be washed. Further, the reflux block 4 and the reaction block 5 themselves can be washed. After washing, the reaction vessel of the automatic synthesizer can be assembled by inserting the reflux vessel 2 into the reflux block 4 and inserting the reaction vessel 3 into the reaction block 5 again.
[0058]
By the same procedure as the above washing, only a damaged or contaminated reflux vessel or reaction vessel can be replaced with a normal vessel. The pressure adjusting means of the present invention has a structure in which a reaction block or a discharge container is used as a flow path, and does not cause interference with other components of the automatic synthesizer. And can be exchanged.
[0059]
In addition, the formation position of the flow path in the reaction block and the formation position of the flow path in the discharge container can be arbitrary.
[0060]
【The invention's effect】
As described above, according to the automatic synthesizer of the present invention, discharge control such as prevention of discharge of contents in the reaction vessel and promotion of discharge can be performed. Leakage due to expansion or vaporization can be prevented.
[Brief description of the drawings]
FIG. 1 is a perspective view for explaining a configuration of an automatic synthesizer including a pressurizing unit according to a first embodiment.
FIG. 2 is a cross-sectional view for explaining one configuration of an automatic synthesizer including a pressurizing unit according to the first embodiment.
FIG. 3 is a perspective view for explaining a configuration of an automatic synthesizer including a pressurizing unit according to a second embodiment.
FIG. 4 is a partially cutaway perspective view for explaining the outline of the automatic synthesizer of the present invention.
FIG. 5 is a diagram for explaining leakage of contents.

Claims (1)

化学反応により化合物を合成する自動合成機において、
反応容器を着脱可能とする収納部を有する反応ブロックと、
反応容器内の内容物を排出する排出容器と、
前記反応ブロックと排出容器とで形成される密閉空間内の圧力を調整する圧力調整手段を備え、
前記反応容器は、一端を当該反応容器内に通し、他端を前記底部よりも下方位置で排出容器側に開放し、前記両端部分の間に両端の位置よりも高い部分を有し、当該反応容器の内部と外部とを連通する導出管を備え、
前記圧力調整手段は、ガス供給源から密閉空間内にガスを導入して加圧して圧力を高め、当該加圧によって反応容器からの内容物の排出を抑制する自動合成機。In an automatic synthesizer that synthesizes compounds by chemical reaction,
A reaction block having a storage section that allows the reaction vessel to be attached and detached;
A discharge container for discharging the contents in the reaction container;
Pressure adjusting means for adjusting the pressure in the sealed space formed by the reaction block and the discharge container;
The reaction vessel has one end passed through the reaction vessel, the other end opened to the discharge vessel side at a position lower than the bottom, and has a portion higher than the positions at both ends between the both end portions. It has a lead-out pipe that communicates the inside and outside of the container,
The pressure adjusting means is an automatic synthesizer that introduces gas into a sealed space from a gas supply source and pressurizes it to increase the pressure and suppress discharge of contents from the reaction vessel by the pressurization.
JP26954498A 1998-09-24 1998-09-24 Automatic synthesizer Expired - Fee Related JP4569850B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP26954498A JP4569850B2 (en) 1998-09-24 1998-09-24 Automatic synthesizer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP26954498A JP4569850B2 (en) 1998-09-24 1998-09-24 Automatic synthesizer

Publications (2)

Publication Number Publication Date
JP2000093787A JP2000093787A (en) 2000-04-04
JP4569850B2 true JP4569850B2 (en) 2010-10-27

Family

ID=17473867

Family Applications (1)

Application Number Title Priority Date Filing Date
JP26954498A Expired - Fee Related JP4569850B2 (en) 1998-09-24 1998-09-24 Automatic synthesizer

Country Status (1)

Country Link
JP (1) JP4569850B2 (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08506813A (en) * 1993-02-11 1996-07-23 ユニバーシィティー オブ ジョージア リサーチ ファウンデーション，インコーポレイテッド Automated synthesis of oligonucleotides
WO1997010896A1 (en) * 1995-09-22 1997-03-27 Berlex Laboratories, Inc. Apparatus and process for multiple chemical reactions
JPH11292798A (en) * 1998-04-13 1999-10-26 Toyo Eng Corp Apparatus for synthesizing sample

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06138128A (en) * 1992-10-29 1994-05-20 Shimadzu Corp Preparative isolation apparatus
US5609826A (en) * 1995-04-17 1997-03-11 Ontogen Corporation Methods and apparatus for the generation of chemical libraries
WO1998035753A1 (en) * 1997-02-17 1998-08-20 GESELLSCHAFT FüR BIOTECHNOLOGISCHE FORSCHUNG MBH (GBF) Automated chemical synthesis device
JP3066862B2 (en) * 1997-09-30 2000-07-17 株式会社島津製作所 Automatic synthesizer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08506813A (en) * 1993-02-11 1996-07-23 ユニバーシィティー オブ ジョージア リサーチ ファウンデーション，インコーポレイテッド Automated synthesis of oligonucleotides
WO1997010896A1 (en) * 1995-09-22 1997-03-27 Berlex Laboratories, Inc. Apparatus and process for multiple chemical reactions
JPH11292798A (en) * 1998-04-13 1999-10-26 Toyo Eng Corp Apparatus for synthesizing sample

Also Published As

Publication number Publication date
JP2000093787A (en) 2000-04-04

Similar Documents

Publication Publication Date Title
US5417768A (en) Method of cleaning workpiece with solvent and then with liquid carbon dioxide
US5160542A (en) Apparatus for vaporizing and supplying organometal compounds
US5080845A (en) Method of removing impurities from polymeric synthetic plastics materials and an apparatus for carrying out the method
US7431900B2 (en) Hydrogen peroxide vapor system with replaceable desiccant cartridge
KR20010047128A (en) Method of vaporizing a liquid source and apparatus used therefor
JP4569850B2 (en) Automatic synthesizer
JP2000249058A (en) Trap device
US5680961A (en) Configurable system for supplying molten thermoplastic material
KR940004739A (en) Substrate Drying Equipment
FR2915706A1 (en) METHOD FOR MANUFACTURING A LIQUID RESERVOIR USING A BYPASS AND LIQUID TANK
KR960701235A (en) APPARATUS AND METHOD FOR DELIVERING REAGENTS IN VAPOR FORM TO A CVD REACTOR
KR100520417B1 (en) Steam raw material supply system
JP2670830B2 (en) Blow cartridge used to blow a gas into a high temperature liquid, gas discharge assembly and gas blow nozzle using the same, gas blow device and metal pouring device
JP3066862B2 (en) Automatic synthesizer
RU2163218C2 (en) Method of injection or working liquid into microinjection device
RU95121097A (en) METHOD AND APPARATUS FOR ISOLATION OF SUBSTANCE FROM LIQUID MIXTURE BY FRACTIONAL CRYSTALLIZATION
EP0400965A2 (en) Reagent reactor
JP2002292324A (en) Adhesive applying device and method of using the same
US6149869A (en) Chemical synthesizers
US6161300A (en) Alcohol vapor dryer system
US5423921A (en) Method and apparatus for cleaning textiles
JP2002514132A (en) Solid-phase organic synthesis device with pressure regulating manifold
EP0514860B1 (en) Expanding apparatus for agricultural product such as tobacco material
US5268132A (en) Process and device for drawing off and blocking off a melt
JPH1133392A (en) Reaction container

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20041206

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20070921

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20070928

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20071105

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20090528

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20090715

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20100716

A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20100729

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130820

Year of fee payment: 3

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130820

Year of fee payment: 3

LAPS Cancellation because of no payment of annual fees