Method of preparing 4-hydroxy pyrrolidone-2-acetamine
A technology for hydroxypyrrolidone and pyrrolidone, which is applied in the field of preparing 4-hydroxypyrrolidone-2-acetamide, can solve the problems that the purity cannot be fully used for medicine, cannot meet the requirements of industrial scale production, and the product composition is complicated, and the raw materials are cheap and the cost is achieved. Low cost, easy availability of raw materials
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[0029] 1, Preparation of ethyl 4-azidoacetoacetate
[0030] 1000 ml of N,N-dimethylformamide and 167 g (1.0 mol, purity 98.5%) of ethyl 4-chloroacetoacetate were added to the reactor. Sodium azide 110g (2.0mol). The mixture was heated to 100-110°C while stirring, and reacted for 2 hours. After the reaction, the reaction mixture was cooled, and the solvent N,N-dimethylformamide was distilled and recovered under reduced pressure. Add 1000ml of water to the distillation residue, and extract with 1200ml of ethyl acetate (divided into three times, successively 600ml, 400ml, 200ml), combine several times of ethyl acetate, dry with anhydrous magnesium sulfate, and recover ethyl acetate by distillation under reduced pressure. The remainder is ethyl 4-azidoacetoacetate.
[0031] 2, Preparation of 4-hydroxyl-2-pyrrolidone
[0032] Dissolve the ethyl 4-azidoacetoacetate synthesized above in 1000ml of methanol, heat while stirring, control the temperature of the reaction mixture at 40...
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