Synthesis process of thiothiamine

A technology of thiothiamine and synthesis process, which is applied in the direction of organic chemistry, can solve the problems of strong odor, troublesome separation operation, high labor intensity, etc., and achieve the effect of simple process steps, avoiding production cost and reducing waste

Inactive Publication Date: 2014-11-12
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein thiothiamine is an important intermediate for the synthesis of vitamin B1 by this method, and the above-mentioned preparation method has the following defects: 1. In the preparation process of pyrimidine, after the cyclization, it needs to be filtered and dried, that is, to separate the solid from the liquid. The operatio

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Free acetamidine hydrochloride with liquid sodium methylate, then filter, leave the filtered solution, put the solution into a reactor, and add α-(o-chloroaniline) methine-β in the reactor – mass of formamidopropionitrile (enamine), said liquid sodium methoxide, said acetamidine hydrochloride and said α-(o-chloroaniline) methine-β-formamidopropionitrile (enamine) The ratio is 4:2:3, and then the methanol is recovered and the cyclization reaction is carried out under the vacuum pressure of -0.06MPa and the temperature of 50 degrees Celsius. The cyclization reaction time is 2 hours, and the cyclization liquid is obtained.

[0032] Add water to carry out steam distillation in described cyclization liquid, the add-on of described water is 3.5% of the add-on of above-mentioned α-(o-chloroaniline) group methine-beta-formamidopropionitrile (enamine) times, the temperature of the steam distillation is 120 degrees centigrade, and then condensed to the upper and lower layers of t...

Embodiment 2

[0037] Free acetamidine hydrochloride with liquid sodium methylate, then filter, leave the filtered solution, put the solution into a reactor, and add α-(o-chloroaniline) methine-β in the reactor – mass of formamidopropionitrile (enamine), said liquid sodium methoxide, said acetamidine hydrochloride and said α-(o-chloroaniline) methine-β-formamidopropionitrile (enamine) The ratio is 4:2:3, and then the methanol is recovered and the cyclization reaction is carried out under the vacuum pressure of -0.09MPa and the temperature of 100 degrees Celsius. The cyclization reaction time is 4 hours, and the cyclization liquid is obtained.

[0038] Add water and carry out steam distillation in described cyclization liquid, the add-on of described water is described in step (1) α-(o-chloroaniline) base methine-β-formamidopropionitrile (enamine ) 4 times of the add-on, the temperature of the steam distillation is 120 degrees centigrade, then condensed to the upper and lower layers of the solu...

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Abstract

The invention discloses a synthesis process of thiothiamine. The synthesis process comprises the following steps of dissociating acetamidine hydrochloride with liquid sodium methoxide and then filtering to retain the solution, placing the solution into a reactor, adding alpha-(o-chloroaniline)ylmethenyl-beta-formylaminopropionitrile (enamine), and then recovering methanol and carrying out cyclization reaction to obtain a cyclized solution; adding an aqueous phase to the cyclized solution, distilling, wherein the distillation temperature of vapor is 120 DEG C; after o-chloroaniline is completely stripped out, adding a caustic soda liquid, hydrolyzing and then adding water, adding carbon disulfide, reacting, finally adding gamma-chloro-gamma-acetyl propanol, carrying out condensation and filtering to obtain a thiothiamine crude; dissolving with hydrochloric acid, reacting, adding activated carbon, decolorizing, filtering to remain filtrate, neutralizing with the caustic soda liquid; and after a solid is precipitated, filtering and drying the solid to obtain the finished thiothiamine. The synthesis process of thiothiamine disclosed by the invention has the advantages that the process steps are simple, the yield of thiothiamine is high, the generation of wastes is reduced, the environment friendliness is achieved and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of vitamin production, in particular to a synthesis process of thiothiamine. Background technique [0002] The synthetic technology of vitamin B1 at home and abroad, at present relatively mature routes mainly include acrylonitrile acetylpyrimidine route, acrylonitrile formyl pyrimidine route and malononitrile route. In China, the acrylonitrile formyl pyrimidine route is generally used to synthesize vitamin B1. This method mainly includes aminopropionitrile, sodium substitution, enamine, pyrimidine, chlorate, ether hydrochloride, thiothiamine, thiothiamine oxidation, sulfuric acid nitric acid, and sulfuric acid. Amine neutralization, and thiamine hydrochloride and other processes. Wherein thiothiamine is an important intermediate for the synthesis of vitamin B1 by this method, and the above-mentioned preparation method has the following defects: 1. In the preparation process of pyrimidine, after the cyclizat...

Claims

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Application Information

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IPC IPC(8): C07D417/06
CPCC07D417/06
Inventor 李来成沈银元陈英明崔胜凯
Owner 江苏兄弟维生素有限公司
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