摘要
以2-氨基-5-氟苯甲酸为原料,经溴代、重氮化、还原合成中间体3-溴-5-氟苯甲酸,再以甲苯为溶剂,氯化亚砜氯化后通入氨气,所得酰胺和五氧化二磷共热蒸馏得标题化合物,总收率53.4%(以2-氨基-5-氟苯甲酸计)。
3-Bromo-5-fluorobenzonitrile was synthesized from 2-amino-5-fluorobenzoic acid. It started from bromination using 1,3-dibromo-5,5-dimethylhydantoin, dizotization by so- dium nitrite and reduction with ethanol to give 3-bromo-5-fluorobenzonic acid as the key intermediate. Then, the process was followed by chlorination with thionyl chloride, ammonization with ammonia gas in the present of toluene and distillation with phosphorus pentoxide. The overall yield was 53.4% ( based on 2-amino-5-fluorobenzoie acid).
出处
《化学试剂》
CAS
CSCD
北大核心
2013年第12期1143-1145,共3页
Chemical Reagents
基金
国家自然科学基金资助项目(21006010)
2013江苏省大学生实践创新计划资助项目(201313102014YB)