RU2015138428A - Способ очистки неочищенного pnpnh-соединения - Google Patents
Способ очистки неочищенного pnpnh-соединения Download PDFInfo
- Publication number
- RU2015138428A RU2015138428A RU2015138428A RU2015138428A RU2015138428A RU 2015138428 A RU2015138428 A RU 2015138428A RU 2015138428 A RU2015138428 A RU 2015138428A RU 2015138428 A RU2015138428 A RU 2015138428A RU 2015138428 A RU2015138428 A RU 2015138428A
- Authority
- RU
- Russia
- Prior art keywords
- alcohol
- stage
- pnpnh
- pnpnh compound
- compound
- Prior art date
Links
- 150000001875 compounds Chemical class 0.000 title claims 11
- 238000000034 method Methods 0.000 title claims 10
- 238000004140 cleaning Methods 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 6
- 125000004122 cyclic group Chemical group 0.000 claims 3
- 238000001035 drying Methods 0.000 claims 3
- 125000000217 alkyl group Chemical group 0.000 claims 2
- 125000003118 aryl group Chemical group 0.000 claims 2
- 239000003446 ligand Substances 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 2
- -1 amino, trimethylsilyl Chemical group 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- 229910052736 halogen Inorganic materials 0.000 claims 1
- 150000002367 halogens Chemical class 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 125000004433 nitrogen atom Chemical group N* 0.000 claims 1
- 125000004437 phosphorous atom Chemical group 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 claims 1
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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
- B01J31/14—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
- C07F9/505—Preparation; Separation; Purification; Stabilisation
- C07F9/5095—Separation; Purification; Stabilisation
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
- B01J31/14—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron
- B01J31/143—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron of aluminium
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/189—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms containing both nitrogen and phosphorus as complexing atoms, including e.g. phosphino moieties, in one at least bidentate or bridging ligand
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
-
- 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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/20—Olefin oligomerisation or telomerisation
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/60—Complexes comprising metals of Group VI (VIA or VIB) as the central metal
- B01J2531/62—Chromium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Saccharide Compounds (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Claims (19)
1. Способ очистки неочищенного PNPNH-соединения общей структуры
R1R2P-N(R3)-P(R4)-N(R5)-H,
где R1, R2, R3, R4 и R5 независимо представляют собой галоген, амино, триметилсилил, C1-С10-алкил, замещенный C1-С10-алкил, С6-С20-арил и замещенный С6-С20-арил или любое циклическое производное, в котором по меньшей мере один из атомов Р или N структуры PNPN-H представляет собой член кольцевой системы, причем кольцевая система образована замещением из одного или нескольких соединений-компонентов PNPNH-структуры,
включающий стадии:
А.
a) растворения неочищенного PNPNH-соединения в C1-С10-спирте или их смеси при нагревании, при этом массовое соотношение спирт/лиганд составляет 5,0-0,1, предпочтительно 1,0-0,3;
b) охлаждения раствора, полученного на стадии а), и
c) выделения PNPNH-соединения, предпочтительно осаждением PNPNH-соединения из раствора, отделения PNPNH-соединения от раствора и необязательно сушки PNPNH-соединения, или
В.
(i) промывки неочищенного PNPNH-соединения C1-С10-спиртом или их смесью;
(ii) отделения PNPNH-соединения и необязательно его сушки.
2. Способ по п. 1, в котором неочищенное PNPNH-соединение растворяют на стадии а) в или промывают на стадии (i) C1-C5-спиртом, предпочтительно этанолом.
3. Способ по п. 1 или 2, в котором массовое соотношение спирт/лиганд на стадии (i) составляет 5,0-0,1, предпочтительно 1,0-0,3.
4. Способ по п. 1 или 2, в котором нагревание на стадии а) проводят до температуры приблизительно 50-100°C.
5. Способ по п. 1 или 2, в котором раствор на стадии b) охлаждают до температуры от -20 до +20°C, предпочтительно от 0 до 10°C.
6. Способ по п. 1 или 2, в котором зародыши кристаллов PNPNH добавляют перед или во время стадии b) и/или c).
7. Способ по п. 1 или 2, в котором осадок, полученный на стадии с), промывают С1-С5-спиртом предпочтительно при температуре 0-25°C, и затем сушат при 10-50°C, предпочтительно 15-25°C, под вакуумом 5,0-500 миллибар, предпочтительно 10-100 миллибар.
8. Способ по п. 1 или 2, в котором промывку на стадии i) проводят при температуре приблизительно 0-25°C, предпочтительно 15-25°C.
9. Способ по п. 1 или 2, в котором C1-С10-спирт удаляют на стадии ii) сушкой при 10-50°C, предпочтительно 15-25°C, под вакуумом 5,0-500 миллибар, предпочтительно 10-100 миллибар.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP13154794.5 | 2013-02-11 | ||
| EP13154794.5A EP2764915B1 (en) | 2013-02-11 | 2013-02-11 | Purification method for a crude PNPNH compound |
| PCT/IB2014/058919 WO2014122633A1 (en) | 2013-02-11 | 2014-02-11 | Method for purifying a crude pnpnh compound |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| RU2015138428A true RU2015138428A (ru) | 2017-03-16 |
| RU2659038C2 RU2659038C2 (ru) | 2018-06-27 |
Family
ID=47666058
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| RU2015138428A RU2659038C2 (ru) | 2013-02-11 | 2014-02-11 | Способ очистки неочищенного pnpnh-соединения |
Country Status (14)
| Country | Link |
|---|---|
| US (1) | US9206207B2 (ru) |
| EP (2) | EP2764915B1 (ru) |
| JP (1) | JP6309029B2 (ru) |
| KR (1) | KR102194647B1 (ru) |
| CN (1) | CN104981291B (ru) |
| BR (1) | BR112015019129B1 (ru) |
| CA (1) | CA2899217C (ru) |
| ES (2) | ES2624430T3 (ru) |
| MX (1) | MX367211B (ru) |
| MY (1) | MY169853A (ru) |
| RU (1) | RU2659038C2 (ru) |
| SG (1) | SG11201505430UA (ru) |
| TW (1) | TWI634946B (ru) |
| WO (1) | WO2014122633A1 (ru) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2764913A1 (en) | 2013-02-11 | 2014-08-13 | Linde AG | Method for purifying a crude PNPNH compound |
| EP2764914A1 (en) | 2013-02-11 | 2014-08-13 | Linde AG | Metalated PNPNH ligand, catalyst composition and use thereof in the oligomerization of ethylene |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0895811A1 (en) * | 1997-08-08 | 1999-02-10 | Dsm N.V. | Process to separate a group 8-10 metal/phosphite ligand complex from an organic liquid |
| GC0000291A (en) * | 2000-06-30 | 2006-11-01 | Shell Int Research | Ligands and catalyst systems thereof for ethylene oligomerisation to linear alpha olefins |
| GB0016895D0 (en) | 2000-07-11 | 2000-08-30 | Bp Chem Int Ltd | Olefin oligomerisation |
| TWI307696B (en) * | 2006-03-02 | 2009-03-21 | San Fu Chemical Co Ltd | Process for purifying sucralose |
| RU2456078C2 (ru) | 2007-07-11 | 2012-07-20 | Линде Аг | Каталитическая композиция и способ ди-, три- и/или тетрамеризации этилена |
| ES2371218T3 (es) | 2009-04-09 | 2011-12-28 | Saudi Basic Industries Corporation | Composición de catalizador y procedimiento para la oligomerización de etileno. |
| EP2764913A1 (en) | 2013-02-11 | 2014-08-13 | Linde AG | Method for purifying a crude PNPNH compound |
| EP2764914A1 (en) | 2013-02-11 | 2014-08-13 | Linde AG | Metalated PNPNH ligand, catalyst composition and use thereof in the oligomerization of ethylene |
-
2013
- 2013-02-11 ES ES13154794.5T patent/ES2624430T3/es active Active
- 2013-02-11 EP EP13154794.5A patent/EP2764915B1/en active Active
-
2014
- 2014-02-10 TW TW103104269A patent/TWI634946B/zh not_active IP Right Cessation
- 2014-02-10 US US14/176,609 patent/US9206207B2/en active Active
- 2014-02-11 SG SG11201505430UA patent/SG11201505430UA/en unknown
- 2014-02-11 WO PCT/IB2014/058919 patent/WO2014122633A1/en active Application Filing
- 2014-02-11 MY MYPI2015001822A patent/MY169853A/en unknown
- 2014-02-11 CN CN201480008408.1A patent/CN104981291B/zh active Active
- 2014-02-11 JP JP2015556610A patent/JP6309029B2/ja active Active
- 2014-02-11 MX MX2015010324A patent/MX367211B/es active IP Right Grant
- 2014-02-11 EP EP14707242.5A patent/EP2953718B1/en active Active
- 2014-02-11 KR KR1020157022961A patent/KR102194647B1/ko active IP Right Grant
- 2014-02-11 ES ES14707242T patent/ES2865133T3/es active Active
- 2014-02-11 BR BR112015019129-0A patent/BR112015019129B1/pt not_active IP Right Cessation
- 2014-02-11 RU RU2015138428A patent/RU2659038C2/ru active
- 2014-02-11 CA CA2899217A patent/CA2899217C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP6309029B2 (ja) | 2018-04-11 |
| KR20150117277A (ko) | 2015-10-19 |
| SG11201505430UA (en) | 2015-08-28 |
| ES2624430T3 (es) | 2017-07-14 |
| TWI634946B (zh) | 2018-09-11 |
| US20140228594A1 (en) | 2014-08-14 |
| EP2764915B1 (en) | 2017-03-22 |
| JP2016509992A (ja) | 2016-04-04 |
| CA2899217A1 (en) | 2014-08-14 |
| CN104981291B (zh) | 2018-03-23 |
| ES2865133T3 (es) | 2021-10-15 |
| US9206207B2 (en) | 2015-12-08 |
| MX367211B (es) | 2019-08-08 |
| BR112015019129B1 (pt) | 2020-12-15 |
| WO2014122633A1 (en) | 2014-08-14 |
| CN104981291A (zh) | 2015-10-14 |
| BR112015019129A2 (pt) | 2017-07-18 |
| MX2015010324A (es) | 2015-10-26 |
| EP2953718A1 (en) | 2015-12-16 |
| RU2659038C2 (ru) | 2018-06-27 |
| MY169853A (en) | 2019-05-17 |
| KR102194647B1 (ko) | 2020-12-24 |
| CA2899217C (en) | 2018-11-20 |
| EP2764915A1 (en) | 2014-08-13 |
| TW201446327A (zh) | 2014-12-16 |
| EP2953718B1 (en) | 2021-04-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103012846B (zh) | 一种磷杂菲衍生物阻燃剂 | |
| JP2015527363A5 (ru) | ||
| JP2014532653A5 (ru) | ||
| JP2008515831A5 (ru) | ||
| JP2011173893A5 (ja) | 新規な化合物を含む組成物 | |
| JP2015532645A5 (ru) | ||
| AR062715A1 (es) | Procesos para la preparacion de acidos de 1,2,4- oxadiazol benzoico | |
| PE20141264A1 (es) | Procedimiento de obtencion de una composicion que contiene factores de crecimiento a partir de un compuesto sanguineo, y composicion obtenible por dicho procedimiento | |
| EA201600241A1 (ru) | Замещенные (2r,3r,5r)-3-гидрокси-(5-пиримидин-1-ил)тетрагидрофуран-2-илметил арил фосфорамидаты | |
| RU2011106794A (ru) | Способы экстракции и очистки промежуточного продукта получения сукралозы | |
| RU2015138503A (ru) | Способ экстракции и выделения | |
| JP2012001634A5 (ru) | ||
| RU2015138428A (ru) | Способ очистки неочищенного pnpnh-соединения | |
| RU2013138356A (ru) | Способ крупномасштабного получения протеогликана | |
| RU2017119446A (ru) | Способ получения изоцианата | |
| RU2016111704A (ru) | Производные дезоксинойиримицина и способы их применения | |
| CO6700138A1 (es) | Procedimiento de preparación de sal de l-arginina de perindoprilo | |
| EA201790710A1 (ru) | Способ получения глатирамера ацетата | |
| RU2016107486A (ru) | Способ получения рифаксимина к | |
| AR081267A1 (es) | Procedimiento de obtencion de la forma cristalina a del febuxostat | |
| UA112623C2 (uk) | Розгалужені олігоарилсилани та спосіб їх отримання | |
| JP2010512392A5 (ru) | ||
| RU2011152457A (ru) | Способ очистки нитрата калия | |
| RU2013122374A (ru) | Препарат, обладающий антитоксической активностью и содержащий комплексное соединение производного метилурацила с органической кислотой, и способ его получения | |
| RU2015138427A (ru) | Способ очистки неочищенного pnpnh-соединения |