Synthetic method of 2-methyl-4-amino-5-formyl aminomethylpyrimidine

Abstract

The invention relates to a synthetic method of 2-methyl-4-amino-5-formyl aminomethylpyrimidine. The method comprises the following steps: a benzene solvent and a solid acid catalyst are added to a reaction flask and stirred, alpha-sodio formyl-beta-formyl aminopropionitrile is added, heating is performed, an acetamidine hydrochloride solution dissolved in an alcohol solvent is added dropwise, a thermal reaction and filtering are performed, the solid acid catalyst is recovered and treated for recycling, and a filtrate is a 2-methyl-4-amino-5-formyl aminomethylpyrimidine solution. O-chloroaniline as a raw material used in the traditional synthetic process is not used, 2-methyl-4-amino-5-formyl aminomethylpyrimidine is directly synthesized from alpha-sodio formyl-beta-formyl aminopropionitrile and acetamidine hydrochloride under the action of the solid acid catalyst, intermediate processes are omitted, the method is an environment-friendly process because the solid acid catalyst is recyclable, and trace cancerogen residues in a vitamin B1 product are avoided; synthesis yield is high, and the requirement for current green development is met.

Description

technical field [0001] The invention relates to a convenient synthesis method of 2-methyl-4-amino-5-formylaminomethylpyrimidine, a key intermediate of vitamin B1, and belongs to the technical field of synthesis of vitamin B1 and its derivatives. Background technique [0002] 2-Methyl-4-amino-5-formylaminomethylpyrimidine is a key intermediate for the synthesis of vitamin B1, the method of synthesizing 2-methyl-4-amino-5-formylaminomethylpyrimidine reported at home and abroad Have: [0003] Chinese patent CN103012282A discloses using α-sodioformyl-β-formamidopropionitrile II as the starting material, and the steps for synthesizing 2-methyl-4-amino-5-formylaminomethylpyrimidine are three steps: 1) II reacts with hydrogen chloride gas to prepare α-enol-β-formamidopropionitrile; 2) acetamidine hydrochloride is dissociated into acetamidine; 3) α-enol-β-formamidopropionitrile reacts with free acetamidine Amidine cyclization system I. This synthetic method has a long route and al...

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Problems solved by technology

[0003] Chinese patent CN103012282A discloses using α-sodioformyl-β-formamidopropionitrile II as the starting material, and the steps for synthesizing 2-methyl-4-amino-5-formylaminomethylpyrimidine are three steps: 1) II reacts with hydrogen chloride gas to prepare α-enol-β-formamidopropionitrile; 2) acetamidine hydrochloride is dissociated into acetamidine; 3) α-enol-β-formamidopropionitrile reacts with free acetamidine Amidine cyclization system I. This synthetic method route is long, also needs to use hydrogen chloride and sodium methylate, and the by-product sodium chloride is produced more in the process

However, o-chloroaniline is a carcinogen and will have trace residues in vitamin B1 products

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