N-(4-苯甲氰基)-3-氯苯甲酰胺的合成工艺研究 |
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引用本文: | 李凤琼,穆敏婕,张梅,师健友.N-(4-苯甲氰基)-3-氯苯甲酰胺的合成工艺研究[J].成都电子机械高等专科学校学报,2015(4):73-75. |
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作者姓名: | 李凤琼 穆敏婕 张梅 师健友 |
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作者单位: | 1. 成都中医药大学药学院,中药材标准化教育部重点实验室,中药资源系统研究与开发利用省部共建国家重点实验室培育基地,成都 611137;2. 四川省医学科学院? 四川省人民医院,成都,610072 |
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基金项目: | 四川省卫计委课题,四川省卫计委课题 |
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摘 要: | 为了得到合成 N-(4-苯甲氰基)-3-氯苯甲酰胺的最优条件,以3-氯苯甲酸和4-硝基苯甲腈为起始原料,经还原、酰氯化、酰胺化合成 N-(4-苯甲氰基)-3-氯苯甲酰胺,考察不同反应条件对产品收率的影响。实验结果表明,得出最佳反应条件为:3-氯苯甲酸与4-氨基苯甲腈物料比1∶1.15,滴加过程控温0~5℃,缚酸剂:DIEA,用量为胺的2倍量,反应2 h,产品收率为89%。得出结论:建立了一种合成 N-(4-苯甲氰基)-3-氯苯甲酰胺的合成路线,该合成路线反应条件温和、工艺操作简便、容易控制。
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关 键 词: | 3-氯苯甲酸 4-硝基苯甲腈 还原 酰氯 |
The Synthesis of 3-Chloro-N-(4-Cyanophenyl) Benzamide |
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Abstract: | To get an optimal condition for the synthesis of 3-chloro-N-( 4-cyanophenyl) benzamide,3-chloro-N-( 4-cyanophenyl) benzamide was synthesized from 4-nitrobenzonitrile and 3-chlorobenzoic acid by reduction, chloride, amide.The effect of different reaction conditions on product yield was investigated.The target compound could be obtained in 89% by the best condition: 3-chloro-benzoic acid with 4-aminobenzonitrile material ratio of 1∶1.15, dropping temperature 0 ~5 ℃, acid binding agent: N,N-Diisopropylethylamine, in an amount of 2-times amount of amine,reaction for two hours.A synthesis route was established for the synthesis of 3-chloro-N-(4-cyanophenyl) benzamide, the synthetic route is in mild reaction conditions, the process is simple to operate, easy to control. |
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Keywords: | 3-chlorobenzoic acid 4-nitrobenzonitrile reduction chloride |
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