N-苯基碳酰胺酸甲酯的合成

研讨了N-苯基甲酰胺酸甲酯（MPC）的新颖合成,整个合成分为两步完成：①起始原料尿素与苯胺在无溶剂存在下反应合成N,N′-二苯基脲（DPU）,通过实验确定最佳工艺条件为：反应温度170℃;n（苯胺）∶n（尿素）=5∶1;反应时间1.5h,N,N′-二苯基脲粗产物经重结晶法纯化,产率可达96.3%;②N,N′-二苯基脲与甲醇在高压反应釜中（氮气保护）无其它溶剂存在下醇解反应合成N-苯基碳酰胺酸甲酯。经过实验优化确定反应工艺条件为：反应温度170℃,n（N,N′-二苯基脲）∶n（甲醇）=1∶10,反应时间4h。粗产物经柱色谱分离提纯,N-苯基碳酰胺酸甲酯的分离产率可达83.7%。所有产物的分子结构经1 H NMR,13C NMR以及IR光谱表征。

A Study on the Synthesis of Methyl N-Phenyl Carbamate

A novel synthesis of methyl N-phenyl carbamate was explored in this paper.The whole syntheses were composed of two steps.In the first step,starting materials urea and aniline were reacted neat to afford N,N′-diphenyl urea（DPU）,the optimal conditions were determined by the experiment as follows：reaction temperature 170℃;molar ratio of the reactants n（aniline）∶n（urea）=5∶1;reaction time 1.5h.The crude product N,N′-diphenyl urea was purified by re-crystallization with 96.3%isolated yield;in the second step,N,N′-diphenyl urea underwent alcoholysis with methanol neat in pressure reactor under protective atmosphere of nitrogen to form the target product methyl N-phenyl carbamate（MPC）.The technical conditions were optimized by the experiment as follows：reaction temperature 170 ℃;molar ratio of the reactants n（N,N′-diphenyl urea）∶n（methanol）=1∶10;reaction time 4h. The crude product was purified by column chromatography with 83.7% isolated yield.The molecular structures of all the products were characterized by 1 H NMR,13C NMR and IR spectroscopy respectively.