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3-溴-5-氟苯甲腈的合成

Synthesis of 3-bromo-5-fluorobenzonitrile

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【作者】 贺新邱岳进曹颖秋聂华丽

【Author】 HE Xin;QIU Yue-jin;CAO Ying-qiu;NIE Hua-li;Changzhou Institute of Engineering Technology;Changzhou Entry-Exit Inspection and Quarantine;College of Chemistry,Chemical Engi neering and Biotechnology,Donghua University;

【机构】 常州工程职业技术学院化工系常州出入境检验检疫局东华大学化学化工与生物工程学院

【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).

【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)
  • 【分类号】O625.67
  • 【被引频次】2
  • 【下载频次】192
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