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出 处:《应用化工》2006年第6期414-415,419,共3页Applied Chemical Industry
基 金:江苏省高新技术产业发展项目(JHB05-33)
摘 要:在乙醇钠催化下邻硝基甲苯与草酸二乙酯缩合后,经水解、双氧水氧化、盐酸酸化得到邻硝基苯乙酸,收率为62%。邻硝基苯乙酸再经硫化铵还原、重氮化反应、水解得到苯并呋喃-2(3H)-酮。考察了重氮化反应时间和水解温度对反应的影响,适宜的重氮化反应时间为30 m in,适宜的水解温度135℃,在此条件下苯并呋喃-2(3H)-酮的收率为51%。两步总收率为32%。o-Nitrophenylacetic acid was synthesized by condensation of o-nitrotoluene with diethyl oxalate catalyzed by C2H5ONa, hydrolysis, oxidation with H2O2 and acidation with HC1 in'about 62% yield. It was further converted to benzofuran-2 ( 3 H) -one by reduction with ( NH4 ) 2 S, diazonation and hydrolysis. The reaction time of diazotization and the temperature of hydrolysis were investigated. The results showed that under the conditions of the reaction time of diazonation for 30 rain and the temperature of hydrolysis 135℃ ,the yield of benzofuran-2(3H)-one is about 51%. The overall yield is about 32%.
关 键 词:苯并呋喃-2(3H)-酮 邻硝基甲苯 邻硝基苯乙酸 合成
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