2-甲酰胺环己酮的简便合成

Facile synthesis of cyclohexanone-2-carboxamide

以二甲苯作溶剂,环己酮、碳酸铵和尿素为原料,在无催化条件下,经两步反应制得2-甲酰胺环己酮。研究了聚合反应温度、碳酸铵和二甲苯的用量对产品质量和收率的影响。结果表明,最佳质量比为50∶18∶9∶25的环己酮、尿素、碳酸铵和二甲苯的混合物在137~142℃经聚合反应生成螺环,螺环用9.6%的稀硫酸水解即得产品,总收率54.6%。

Cyclohexanone-2-carboxamide was prepared by two-step process in the absence of catalyst with xylene as solvent,and cyclohexanone,ammonium carbonate and urea as starting materials.The influence of condensation temperature,the dose of ammonium carbonate and xylene on the quality and yield of the product was investigated by orthogonal experiment.The results showed that the optimal mass ratio of cyclohexanone,urea,ammonium carbonate and xylene was 50 ∶18 ∶9 ∶25.Spirolactam was synthesized by condensation reaction with the mixed materials at 137~142 ℃,and then spirolactam was hydrolyzed to cyclohexanone-2-carboxamide in 9.6% H2SO4 solution,and the total yield is 54.6%.