N-(3-氯苯基)金刚烷甲酰胺的合成

Synthesis of N-(3-chlorophenyl)-1-adamantanecarboxamide

以金刚烷和无水甲酸为原料,在浓硫酸催化下合成1-金刚烷甲酸,再经酰化反应生成目标产物,总收率约为85.3%。第2步最佳的工艺条件为:反应温度130℃,反应时间4 h,1-金刚烷甲酸、间氯苯胺和亚磷酸三苯酯的投料物质的量比为1∶1∶0.6,溶剂用量50 mL。所得化合物结构经1H NMR和IR进行表征。

1-Adamantanecarboxyli acid was synthesized by the reaction of adamantine with formic acid in the presence of concentrated sulfuric acid, and subsequently converted to N-（3-chlorophenyl）-1-adamantanecarboxamide,which was subjected to aeylation with an overall yield of about 85.3%. The optimum condition of the third step for the reaction were as follows：the temperature was 130 ℃ ,the reaction time was 4 h,the molar ratio of 1-adamantanecarboxylic acid,3-chloroaniline and triphenyl phosphate was 1 ： 1 ：0.6,the solvent volume of dimethylformamide was 50 mL. These compounds were characterized by ^1H NMR and IR.