摘要
邻氨基苯腈经重氮化、还原、酸析制得邻氰基苯肼盐酸盐。邻氰基苯肼盐酸盐经碱液中和,在乙醇溶液中与乙酰乙酸甲酯的醇溶液经亲核取代闭环成目标产物1-(2-氰基)-苯基-3-甲基-5-吡唑啉酮。对邻氰基苯肼盐酸盐和1-(2-氰基)-苯基-3-甲基-5-吡唑啉酮的合成工艺进行了改进,总收率约为79.4%
1-（2-Cyan）-phenyl-3-methyl-5-pyrazolone is synthesized from 2-aminobenzonitrile by diazotization, reduction with stannous chloride in the presence of hydrochloric acid to give 2-cyanphenylhydrazine hydrochloride, which is subjected to neutralization with sodium methoxide and nucleophilic reaction with methyl acetoacetate. The method has been improved in the process of synthesis of 2-cyanphenylhydrazine hydrochloride and 1-（2-cyan）-phenyl-3-methyl-5-pyrazolone and the total yield can be increased to 79.4%.
出处
《现代化工》
CAS
CSCD
北大核心
2009年第8期56-57,共2页
Modern Chemical Industry
基金
江苏省教育厅自然科学基金资助(08KJA530002)
国家"863"计划项目(2007AA02Z211)
