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Synthetic method of vitamin B1 intermediate

A synthesis method and intermediate technology, which are applied in the field of chemical drug preparation, can solve the problems of large dust, high labor intensity, high energy consumption in the recovery process of o-chloroaniline, etc., and achieve the effect of optimizing technological process and reducing labor intensity.

Active Publication Date: 2013-04-03
HUAZHONG PHARMA
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Problems solved by technology

[0006] In the traditional process, o-chloroaniline, a raw material, is highly toxic, and the recovery process of o-chloroaniline consumes a lot of energy and the recovery rate is low, which is extremely harmful to the human body and the environment.
The intermediate α-(o-chloroaniline)-aminomethyl-β-formamidopropionitrile needs to be dried, which is dusty and labor-intensive

Method used

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  • Synthetic method of vitamin B1 intermediate
  • Synthetic method of vitamin B1 intermediate
  • Synthetic method of vitamin B1 intermediate

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Embodiment Construction

[0018] The present invention is illustrated with examples below, and these examples are intended to help understand technical means of the present invention. However, it should be understood that these embodiments are only exemplary, and the present invention is not limited thereto.

[0019] 1. Preparation of compound α-enolyl-β-formamidopropionitrile (Ⅲ)

[0020] Disperse 68g (0.32mol, content 70%) of α-sodium formyl-β-formamidopropionitrile (IV) in 100g of methanol in a four-neck flask, feed 0.4mol of dry hydrochloric acid gas, and keep the temperature at At about 20°C, react for 1 hour and then filter, the filtrate is 138g of methanol solution of α-enolyl-β-formamidopropionitrile (Ⅲ).

[0021] 2. Preparation of compound acetamidine (Ⅱ)

[0022] Put 50g of acetamidine hydrochloride (0.48mol, content ≥ 91.0%) into a dry three-necked flask, keep warm in a water bath at about 25°C, add 95g of liquid sodium methoxide (0.49mol, content 28%) dropwise with a constant pressure fun...

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Abstract

The invention relates to an improvement of a synthetic method of an important vitamin B1 intermediate 2-methyl-4-amino-5-formyl ammonium methyl pyridine. According to the method provided by the invention, the raw material o-chloroaniline in the prior synthetic process is omitted, the 2-methyl-4-amino-5-formyl ammonium methyl pyridine is synthesized directly by alpha-sodium substituted formyl-beta-formyl amine propionitrile and ethanamidine, so that the middle process is reduced.

Description

technical field [0001] The invention relates to a preparation method of chemical medicine, in particular to an improved synthesis method of 2-methyl-4-amino-5-aminomethylpyrimidine, an important intermediate of vitamin B1. Background technique [0002] The structural formula of 2-methyl-4-amino-5-aminomethylpyrimidine is: [0003] [0004] 2-methyl-4-amino-5-aminomethylpyrimidine is an important intermediate for the synthesis of vitamin B1. Its traditional synthesis process uses α-sodium formyl-β-formamidopropionitrile as raw material, and prepares α-(o-chloroaniline)-aminomethyl-β with o-chloroaniline hydrochloride in aqueous solution -formamidopropionitrile, and then cyclization reaction with free acetamidine under vacuum environment to prepare 2-methyl-4-amino-5-formamidomethylpyrimidine. [0005] [0006] In the traditional process, o-chloroaniline, a raw material, is required. O-chloroaniline is highly toxic, and the recovery process of o-chloroaniline consumes ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/42
Inventor 王勇李新宇付林薛俊安国盾朱珍珍徐勇
Owner HUAZHONG PHARMA
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