CN104693089B - Continuous preparation process method of N-acetate pyrrolidone - Google Patents
Continuous preparation process method of N-acetate pyrrolidone Download PDFInfo
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- CN104693089B CN104693089B CN201510081706.XA CN201510081706A CN104693089B CN 104693089 B CN104693089 B CN 104693089B CN 201510081706 A CN201510081706 A CN 201510081706A CN 104693089 B CN104693089 B CN 104693089B
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- solvent
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- pyrrolidone
- tubular type
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/27—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with substituted hydrocarbon radicals directly attached to the ring nitrogen atom
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
Abstract
The invention discloses a continuous preparation method of N-acetate pyrrolidone. The method comprises the following steps: by taking a tubular salt formation reactor, mixing pyrrolidone or sodium methoxide with a solvent in a raw material mixer (1), then continuously introducing sodium methoxide or pyrrolidone into the tubular salt formation reactor (2) and a reactive distillation tower according to a ratio, distilling a mixture of methyl alcohol and the solvent from the tower top, supplementing the solvent for a tower kettle solution, then continuously introducing the solvent and methyl chloroacetate or ethyl chloroacetate into a tubular condensation reactor (5) according to a ratio, cooling and filtering condensation reactants, recycling the solvent and distilling to prepare N-acetate pyrrolidone. According to the continuous preparation method of N-acetate pyrrolidone, pyrrolidone serves as a starting raw material and is applied to continuous preparation of N-acetate pyrrolidone through salt formation and condensation reaction in a process of preparing acetamide pyrrolidone (piracetam); the tubular salt formation reactor and the tubular condensation reactor with jackets outside and turbulent flow elements inside are excellent in mass transfer effect, full in material contact, high in reaction speed and accurate in control of reaction temperature, thereby facilitating the improvement of the quality of products.
Description
Technical field
The present invention relates to a kind of preparation facilities of medicine intermediate and its using method and in particular to be acetamide pyrroles
The serialization preparation facilities of alkanone (piracetam) intermediate n- pyrrolidone acetate and using method, n- pyrrolidone acetate
Structure as follows:
Background technology
In formula, r is ch3Or c2h5
N- pyrrolidone acetate is the intermediate of Piracetam (piracetam).
Piracetam (piracetam) is a kind of drugs for nervous, plays the role of to promote brain memory function, right
Old Memorability goes down and the intelligence of some mentally handicapped youngsters improves effectively, to brain trauma, cerebrovas-cularaccident, epilepsy sequelae, an oxygen
Change the memory that carbon and alcohol or drug poisoning cause and the disturbance of thought is also effective in cure, be widely used to clinic at present.
The preparation method preparing Piracetam (piracetam) has multiple, comparative maturity and industrialized method
It is with pyrrolidones as initiation material, through becoming salt, condensation, reaction obtains n- pyrrolidone acetate, then is obtained through aminating reaction
Product, preparation process is batch process procedures.
Content of the invention
It is an object of the invention to provide one kind is with pyrrolidones as initiation material, through becoming salt, condensation to prepare acetamide pyrroles
The serialization preparation facilities of alkanone (piracetam) intermediate n- pyrrolidone acetate and use process.
Technical scheme is as follows:
A kind of continuous preparation process method of n- pyrrolidone acetate, described preparation method includes following preparation dress
Put and preparation process:
A. preparation facilities used includes: material mixer, tubular type salt-forming reactor, reactive distillation column, supplementary solvent mix
Clutch, tubular type condensation reactor, equipment room connecting pipeline, control instrument and annex；Material mixer, tubular type salt-forming reactor,
Supplementary solvent blender, tubular type condensation reactor are the tube type apparatus with or without chuck, manage interior setting interior with chuck or do not set
Put the dynamic and static hybrid element having disturbance immixture to material.
B. preparation process used includes: pyrrolidones or sodium methoxide and solvent are through material mixer and sodium methoxide or pyrroles
Alkanone continuously enters tubular type salt-forming reactor in proportion；The material going out tubular type salt-forming reactor enters reactive distillation column, and tower top distillates
Methyl alcohol and solvent mixture；Tower bottoms with supplement solvent through supplement solvent blender mix after with methyl chloroacetate or monoxone second
Ester continuously enters tubular type condensation reactor in proportion；The reactant liquor going out tubular type condensation reactor is cooled, filter, solvent reclaims,
Distill to obtain n- pyrrolidone acetate.
A kind of continuous preparation process method of described n- pyrrolidone acetate, pyrrolidones and solvent meet,
Mixed solvent and the material after sodium methoxide meet, salt-forming reaction with supplement at solvent mixing, mixed material and methyl chloroacetate
Or ethyl chloroacetate meet can arrange jet mixer, another strand of material is aspirated by one material.
A kind of continuous preparation process method of described n- pyrrolidone acetate, tubular type salt-forming reactor, tubular type contracting
Closing reactor can use the reactor that other type can operate continuously to replace.
A kind of continuous preparation process method of described n- pyrrolidone acetate, material mixer, supplementary solvent mix
Clutch can be replaced with other types of mixing arrangement.
A kind of continuous preparation process method of described n- pyrrolidone acetate, reactive distillation column can use conventional distillation
Kettle replaces；
A kind of continuous preparation process method of described n- pyrrolidone acetate, material is in pushing away that each equipment room flows
Power is provided by pump, potential difference, pressure difference；
A kind of continuous preparation process method of described n- pyrrolidone acetate, can before tubular type salt-forming reactor or
The material that can accelerate reaction rate or improve product quality is added before tubular type condensation reactor.
The invention has the advantage that
1. can make to be prepared for initiation material one-tenth salt in Piracetam (piracetam) technique, condensation by pyrrolidones
React n- pyrrolidone acetate processed and realize serialization preparation.
2. adopt peripheral hardware chuck, inside set tubular type salt-forming reactor and the tubular type condensation reactor of turbulent element, mass transfer effect
Good, fully, reaction speed is fast for material contact；Heat-transfer effect is good, and reaction temperature controls precisely, is conducive to improve product quality.
3. combined with tower reactive distillation using pipe reaction, reaction speed can be improved, quick separating goes out the first of generation
Alcohol, is conducive to reaction to carry out to positive direction, and reaction carries out completely, good product quality, and raw material availability is high；
4. process operation is convenient stable, and preparation efficiency is high, and operating flexibility is big.
Brief description
Fig. 1 is to complete salt-forming reaction using tubular type salt-forming reactor, reactive distillation column and separate methyl alcohol；Using tubular type tubular type
Condensation reactor completes condensation reaction, and serialization preparation is obtained the preparation facilities sketch of n- pyrrolidone acetate.
Specific embodiment
Embodiment 1
The serialization preparation facilities of n- pyrrolidone acetate includes material mixer 1, tubular type salt-forming reactor 2, reaction
Rectifying column 3, supplementary solvent blender 4, tubular type condensation reactor 5, equipment room connecting pipeline, control instrument and annex.Raw material mixes
Clutch 1, tubular type salt-forming reactor 2, supplementary solvent blender 4, tubular type condensation reactor 5 are connected by straight tube and curved tube, in straight tube
The tube type apparatus of filling chemical filler；The continuous preparation method of n- pyrrolidone acetate includes pyrrolidones with solvent through former
Material blender 1 continuously enters tubular type salt-forming reactor 2 in proportion with sodium methoxide；The material going out tubular type salt-forming reactor 2 enters reaction
Rectifying column 3, tower top distillates methyl alcohol and solvent mixture；Tower bottoms with supplement solvent through supplement solvent blender 4 mix after with chlorine
Methyl acetate continuously enters tubular type condensation reactor 5 in proportion；The reactant liquor going out tubular type condensation reactor 5 is cooled, filter, molten
Matchmaker reclaims, distills to obtain n- pyrrolidone acetate, and solvent used is toluene, and the raw material participating in condensation reaction is methyl chloroacetate.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is material mixer 1, tubular type salt-forming reactor 2, supplements
Solvent blender 4, tubular type condensation reactor 5 straight length adopt commercially available static mixer, and curved tube section is blank pipe.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, and difference is that in system, two strands of material meets arrange injector,
Another strand of material is aspirated by one material.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 1, and difference is with the distillation still surrogate response essence with agitating device
Evaporate tower 3.
Claims (7)
1. a kind of continuous preparation process method of n- pyrrolidone acetate it is characterised in that described preparation method include with
Lower preparation facilities and preparation method:
Preparation facilities used includes: material mixer (1), tubular type salt-forming reactor (2), reactive distillation column (3), supplementary solvent
Blender (4), tubular type condensation reactor (5), equipment room connecting pipeline, control instrument and annex；Material mixer (1), tubular type
Salt-forming reactor (2), supplement solvent blender (4), tubular type condensation reactor (5) are the tube type apparatus with or without chuck, pipe
Interior and chuck is interior to be arranged or is not provided with the dynamic and static hybrid element having disturbance immixture to material；
Preparation method used includes: pyrrolidones or sodium methoxide mix through material mixer (1) with solvent after with sodium methoxide or
Pyrrolidones continuously enters tubular type salt-forming reactor (2) in proportion；The material going out tubular type salt-forming reactor (2) enters reactive distillation column
(3), tower top distillates methyl alcohol and solvent mixture；Tower bottoms with supplement solvent through supplement solvent blender (4) mix after with chloroethene
Sour methyl esters or ethyl chloroacetate continuously enter tubular type condensation reactor (5) in proportion；Go out the reactant liquor of tubular type condensation reactor (5)
Cooled, filter, solvent reclaim, distill to obtain n- pyrrolidone acetate.
2. a kind of n- pyrrolidone acetate according to claim 1 continuous preparation process method it is characterised in that
Pyrrolidones and solvent meet, mixed solvent and the material after sodium methoxide meet, salt-forming reaction and supplement at solvent mixing,
Mixed material can arrange jet mixer with methyl chloroacetate or ethyl chloroacetate meet, aspirates another strand of thing by one material
Material.
3. a kind of n- pyrrolidone acetate according to claim 1 continuous preparation process method it is characterised in that
Tubular type salt-forming reactor (2), tubular type condensation reactor (5) can use the reactor that other type can operate continuously to replace.
4. a kind of n- pyrrolidone acetate according to claim 1 continuous preparation process method it is characterised in that
Material mixer (1), supplementary solvent blender (4) can use other types of mixing arrangement to replace.
5. a kind of n- pyrrolidone acetate according to claim 1 continuous preparation process method it is characterised in that
Reactive distillation column (3) can use conventional distillation kettle to replace.
6. a kind of n- pyrrolidone acetate according to claim 1 continuous preparation process method it is characterised in that
The motive force that material flows in each equipment room is provided by pump, potential difference, pressure difference.
7. a kind of n- pyrrolidone acetate according to claim 1 continuous preparation process method it is characterised in that
Addition can accelerate reaction rate or improve product quality before tubular type salt-forming reactor (2) or before tubular type condensation reactor (5)
Material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510081706.XA CN104693089B (en) | 2015-02-16 | 2015-02-16 | Continuous preparation process method of N-acetate pyrrolidone |
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| CN201510081706.XA CN104693089B (en) | 2015-02-16 | 2015-02-16 | Continuous preparation process method of N-acetate pyrrolidone |
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| CN104693089A CN104693089A (en) | 2015-06-10 |
| CN104693089B true CN104693089B (en) | 2017-01-18 |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2059619C1 (en) * | 1992-12-08 | 1996-05-10 | Российский научный центр "Прикладная химия" | Method of n-carbethoxymethylpyrrolidone-2 synthesis |
| CN1094485C (en) * | 1999-03-03 | 2002-11-20 | 东北制药总厂 | Process for preparing N-pyrrolidone acetate |
| CN203602531U (en) * | 2013-12-17 | 2014-05-21 | 山东庆云长信化学科技有限公司 | N-methyl pyrrolidone production device |
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