CN105884632A - Medical raw material aminoacetone hydrochloride synthesis method - Google Patents
Medical raw material aminoacetone hydrochloride synthesis method Download PDFInfo
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- CN105884632A CN105884632A CN201410497192.1A CN201410497192A CN105884632A CN 105884632 A CN105884632 A CN 105884632A CN 201410497192 A CN201410497192 A CN 201410497192A CN 105884632 A CN105884632 A CN 105884632A
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- Prior art keywords
- aminoacetone
- raw material
- synthesis method
- hydrochlorate
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- Pyridine Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a practical synthesis method of important medical raw material aminoacetone hydrochloride. Glycine as a raw material, acetic anhydride and pyridine undergo a reaction in a reflux state to produce an acetyl-protected aminoacetone and the acetyl-protected aminoacetone is hydrolyzed to form aminoacetone hydrochloride.
Description
Technical field
The present invention relates to the synthesis of aminoacetone hydrochlorate, aminoacetone hydrochlorate is the initiation material of many pharmaceutical synthesis, the most specific heterocycle
The important intermediate of compound.
Background technology
Aminoacetone hydrochlorate is the initiation material of many pharmaceutical synthesis, the important intermediate of the most specific heterocyclic compound, such as 1, and 3-azoles or 1,3-
Oxazoline compound.
The most domestic synthetic method having no this compound of report.
Summary of the invention
The purpose of the present invention is in order to provide a kind of simple, efficient, reaction method of safety operation, synthesizing amino propanone hydrochloride.
In order to realize said synthesis route, with glycine as raw material, react with acetic anhydride and pyridine at reflux, obtain the second of acetyl group protection
Acylamino-acetone, i.e. compound 1.
Compound 1 adds pyrohydrolysis in hydrochloric acid, it is possible to obtain our desired product aminoacetone hydrochlorate, i.e. compound 2.This crude product pure
Degree can meet general reaction requirement, can direct plunge in application.
The present invention have also discovered a kind of good method of purification, can effectively obtain the sterling of this compound.We optimize various recrystallization condition, finally
Find that alcohols is reasonable recrystallization solvent.
The chemical equation of this anti-invention course of reaction is as follows:
The process conditions of the present invention can be carried out in wider scope, and the reaction condition that the present invention enumerates such as solvent/temperature/reaction ratio/substrate choosing
It is not restrictive for selecting etc., and simply corresponds to the preferred conclusion of the present invention.
The method that will illustrate the present invention by instantiation below.
Detailed description of the invention
Below by following instance, the present invention is further detailed.The synthesis technique that present example is stated is merely illustrative the present invention,
Rather than limitation of the present invention.In the case of the process route of the present invention, present invention process is carried out simple modifications and broadly fall into claimed
Content.
Example one:
In dry 10L reaction bulb, put into glycine 400 grams, pyridine 2.6L, acetic anhydride 5.9L, be then heated to backflow, backflow 6 with right bath
Hour, suitably remove solvent with water pump decompression distillation after cooling, then use oil pump vacuum fractionation, collect 120-125 degree fraction under 50Pa, obtain nothing
Color liquid 360 gram 1, yield 58%.
Example two:
In 3L there-necked flask, put into compound 1 (236 grams), concentrated hydrochloric acid 800mL and water 800mL, be heated to 112 degree and flow through night, water pump next time
After decompression lower removal major part hydrochloric acid, using oil pump decompressing and extracting, gained sticky matter filters with after 300mL isopropanol thermosol, and crystallisation by cooling obtains light
Yellow solid compound 2,93 grams；Yield 43%.
Claims (3)
1. prepare a most succinct method for aminoacetone hydrochlorate, with glycine as raw material, anti-with acetic anhydride and pyridine at reflux
Should, obtain the acetylamino acetone of acetyl group protection；Then hydrolyze and i.e. obtain aminoacetone hydrochlorate.
2. the method for claim 1, it is characterised in that: acetylamino acetone can reduce pressure distilation.
3. the method for claim 1, it is characterised in that: aminoacetone hydrolyzes in hydrochloric acid and i.e. obtains aminoacetone hydrochlorate；And it is permissible
By being recrystallized to give the solid product of high alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410497192.1A CN105884632A (en) | 2014-09-25 | 2014-09-25 | Medical raw material aminoacetone hydrochloride synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410497192.1A CN105884632A (en) | 2014-09-25 | 2014-09-25 | Medical raw material aminoacetone hydrochloride synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105884632A true CN105884632A (en) | 2016-08-24 |
Family
ID=57000058
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410497192.1A Pending CN105884632A (en) | 2014-09-25 | 2014-09-25 | Medical raw material aminoacetone hydrochloride synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105884632A (en) |
-
2014
- 2014-09-25 CN CN201410497192.1A patent/CN105884632A/en active Pending
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160824 |