摘要
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 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.
出处
《常州大学学报（自然科学版）》
CAS
2014年第2期7-10,共4页
Journal of Changzhou University：Natural Science Edition
