取代苯异腈与脂肪胺的加成反应
关键词: 取代苯异腈；脂肪胺；脒；合成
Substituted benzyl isonitrile addition reaction of aliphatic amines
Abstract:This topic uses isonitrile synthesis and fatty amine adduct amidine compounds explored using cyclohexylamine, diisopropylamine isonitrile addition reaction with the optimum conditions for the 15% of the amount of catalyst , the reaction ratio of 1:1.8 , reaction temperature 130 ℃.Substituted aniline with formic acid occurs formylation reaction of the corresponding aniline substituted formyl , then xylene as a solvent , with triethylamine to provide an alkaline environment , with POCl3 as dehydrating agent , the substituted anilide intermediate dehydration iso nitrile, and then adding a catalyst to give the product Cu2O and amidine diethylamine .We obtained by experiment 2 amidine product , N- cyclohexyl-4 - (4 - trifluoromethyl-3 - chlorophenoxy ) benzamidine , a yield of 72% and p-chlorophenyl hexahydro- pyridyl methyl alkylene amine , in 84% yield .These two target compounds were characterized using 1HNMR .
Keywords: Isonitrile substituted benzenes ; aliphatic amines ; squint；synthesis
目录
1 绪论 1
1.1 脒的用途及制备意义 1
1.2 文献综述 5
1.2.1 肟的还原法 5
1.2.2 氨基还原成脒的固相合成 6
1.2.3 催化合成脒法 6
1.2.4 酯合成脒新法 7
1.2.5 改进的Pinner法 8
1.2.6 Sm/TMSCl/H2O(微量)体系法 8
1.2.7酰胺法 9
1.2.8 酮肟法 9
1.2.9羧酸法 10
1.2.10腈的氨解法 10
1.2.11酰胺缩醛法 11
1.2.12原甲酸酯法 11
1.3 本文研究的内容 12
2 实验部分 14
2.1 实验的仪器和试剂 14
2.1.1 实验仪器 14
2.1.2 实验试剂 14
2.2目标化合物的合成 15
2.2.1 对氯甲酰苯胺的制备 15
2.2.2 N-环己基对氯苯脒的制备 15
2.2.3 N,N-二异丙基对氯苯脒的制备 16
2.2.4 对氯苯基吹冰氢吡啶基甲烯基胺的制备 17
2.2.5 N–环己基-4-(4-三氟甲基-3-氯苯氧基)苯脒的制备 17
3 结果与讨论 19
3.1 不同反应条件对生成N-环已基对氯苯脒反应的影响 19
3.1.1 反应时间对生成N-环已基对氯苯脒的影响 19
3.1.2 反应配比对生成N-环已基对氯苯脒的影响 20
3.1.3 反应温度对生成N-环已基对氯苯脒的影响 21
3.1.4 催化剂用量对生成N-环已基对氯苯脒的影响 22
3.2 不同反应条件对生成N,N-二异丙基对氯苯脒反应的影响 23
3.2.1 反应时间对生成N,N-二异丙基对氯苯脒的影响 23
3.2.2 反应配比对生成N,N-二异丙基对氯苯脒的影响 24