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3-溴-5-氟苯甲腈的合成
Synthesis of 3-bromo-5-fluorobenzonitrile
【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)。
【Abstract】 3-Bromo-5-fluorobenzonitrile was synthesized from2-amino-5-fluorobenzoic acid.It started from bromination using 1,3-dibromo-5,5-dimethylhydantoin,dizotization by sodium 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 was53.4%( based on 2-amino-5-fluorobenzoic acid).
【关键词】 3-溴-5-氟苯甲腈;
3-溴-5-氟苯甲酸;
2-氨基-5-氟苯甲酸;
合成;
【Key words】 2-amino-5-fluorobenzoic acid; 3-bromo-5-fluorobenzoic acid; 3-bromo-5-fluorobenzonitrile; synthesis;
【Key words】 2-amino-5-fluorobenzoic acid; 3-bromo-5-fluorobenzoic acid; 3-bromo-5-fluorobenzonitrile; synthesis;
【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)
- 【文献出处】 化学试剂 ,Chemical Reagents , 编辑部邮箱 ,2013年12期
- 【分类号】O625.67
- 【被引频次】2
- 【下载频次】192