2-氨基-5-氯二苯甲酮合成工艺改进  

PROCESS IMPROVEMENT OF 2-AMINO-5-CHLOROBENZOPHENONE

作　　者：张丹丹[1] 王璇[2] 王润南 谭超兰 黄文静[1] 孙雯[3] 张珍明[1,2] 李树安[1] 

机构地区：[1]淮海工学院化工学院,江苏连云港222005 [2]中国矿业大学化工学院,江苏徐州221116 [3]淮海工学院药学院,江苏连云港222005

出　　处：《精细石油化工》2016年第4期43-46,共4页Speciality Petrochemicals

基　　金：国家海洋公益性行业科研专项(201305007);江苏省六大人才高峰资助项目(2009年;2013年);江苏省海洋资源开发研究院科研项目(JSIMR 201409);连云港市工业攻关项目(CG1508)

摘　　要：以苯乙腈和对氯硝基苯为原料经超声辅助法制备5-氯-3-苯基-2,1-苯并异口恶唑,然后经催化氢化和催化转移氢化法分别合成2-氨基-5-氯二苯甲酮,总收率分别为90.0%和88.4%。考察了超声辅助反应及催化氢化还原反应的影响因素。结果表明:当n(苯乙腈)∶n(对氯硝基苯)=1.1∶1,反应时间为1h时,催化氢化还原反应的较佳条件为:5%Pd/C催化剂用量为4%,反应温度20℃,反应时间1h,氢气压力0.1MPa。同时研究了反应机理。Under the condition of ultrasonic,5-chloro-3-phenyl-2,1-benzisoxazole was prepare with pchloronitrobenzene to prepare 5-chloro-3-phenyl-2,1-benzisoxazole,subsequently,5-chloro-3-phenyl-2,1-benzisoxazole respectively generated 2-amino-5-chlorobenzophenone by catalytic hydrogenation using hydrogen gas or ammonium formate in the presence of 5% palladium on carbon with the yield of90.0% and 88.4%in this study.The effects of ultrasound-assisted reaction and catalytic hydrogenation reduction reaction were studied.Under the n（benzyl cyanide）∶n（chloronitrobenzene）=1.1∶1,time of 1h,the optimized conditions of catalytic hydrogenation reduction reaction conditions such as5%Pd/C catalyst dosage of 4%,temperatures of 20 ℃,time of 1h,and hydrogen pressure of0.1 MPa were determined.Meanwhile it studied the reaction mechanism.

关 键 词：2-氨基-5-氯二苯甲酮 苯并异口恶唑 苯乙腈 催化氢化 中间体 

分 类 号：O625.63[理学—有机化学]