Preparation process of 1-n-methyl-2-nitro-5-hydroxymethyl imidazole
AssigneeAscentawits Pharmaceuticals, Ltd.
InventorsZhaoqiang Lu, Jinwei Fan, Qunhui Huang, Yanjun Zhang, Weisu Chen
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AssigneeAscentawits Pharmaceuticals, Ltd.
InventorsZhaoqiang Lu, Jinwei Fan, Qunhui Huang, Yanjun Zhang, Weisu Chen
Estimating the term…
The present invention provides a preparation process of 1-N-methyl-2-nitro-5-hydroxymethylimidazole comprising using N,N′-carbonyldiimidazole and 1-N-methyl-2-aminoimidazole-5-carboxylic acid to react at 45~65° C. for a period of time, and then cooling to 15~25° C. for a period of time until the reaction is complete, and then reacting with a reducing agent to finally obtain 1-N-methyl-2-nitro-5-hydroxymethylimidazole. The present invention uses the relatively safe N,N′-carbonyldiimidazole to replace the highly toxic, strong irritating, strong corrosive, and environmentally demanding isobutyl chloroformate. It has the following advantages: CDI is a solid, non-irritating and non-corrosive, favorable for storage, transportation and environmental protection, low requirements on equipment, and less physical harm to operators; the reaction operation is simple and the post-treatment is simple. The reaction temperature is higher than that of using isobutyl chloroformate, so as to speed up the reaction, save the reaction time and energy consumption. The yield is high, the side reaction is less, and the product is easy to purify: after the reaction is complete, extracting, drying, and concentrating under reduced pressure until it is drained to obtain a high purity product.
A preparation process of 1-N-methyl-2-nitro-5-hydroxymethylimidazole, comprising reacting N,N′-carbonyldiimidazole and 1-N-methyl-2-nitro-5-carboxylic A acid imidazole at 45~65° C. for a period of time, and then cooled to 15~25° C. and reacted for a period of time until the reaction is complete, and then reacted with the reducing agent sodium borohydride or potassium borohydride to finally obtain 1-N-methyl-2-nitro-5-hydroxymethylimidazole.
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