[1]徐崇福,朱建华,郑黄利,等.N苯基碳酰胺酸甲酯的合成[J].常州大学学报(自然科学版),2014,(02):7-10.[doi:10.3969/j.issn.2095-0411.2014.02.003]
　XU Chong-fu,ZHU Jian-hua,ZHENG Huang-li,et al.A Study on the Synthesis of Methyl NPhenyl Carbamate[J].Journal of Changzhou University(Natural Science Edition),2014,(02):7-10.[doi:10.3969/j.issn.2095-0411.2014.02.003]
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N苯基碳酰胺酸甲酯的合成()
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常州大学学报(自然科学版)[ISSN:2095-0411/CN:32-1822/N]

卷:
期数:
2014年02期
页码:
7-10
栏目:
化学化工
出版日期:
2014-04-30

文章信息/Info

Title:
A Study on the Synthesis of Methyl NPhenyl Carbamate
作者:
徐崇福; 朱建华; 郑黄利; 李艺林; 王 颖
常州大学 石油化工学院,江苏 常州 213164
Author(s):
XU Chong-fu; ZHU Jian-hua; ZHENG Huang-li; LI Yi-lin; WANG Ying
School of Petrochemical Engineering,Changzhou University,Changzhou 213164,China
关键词:
N; N′-二苯基脲; N-苯基甲酰胺酸甲酯; 无溶剂反应; 醇解; 压力反应器
Keywords:
N; N'diphenyl urea(DPU);  methyl Nphenyl carbamate(MPC);  neat reaction;  alcoholysis;  pressure reactor
分类号:
O625.6
DOI:
10.3969/j.issn.2095-0411.2014.02.003
文献标志码:
A
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1.5 h,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4 h。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1H NMR,13C NMR 以及IR光谱表征。
Abstract:
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 experimentas follows:reaction temperature 170 ℃; molar ratio of the reactants n(aniline):n(urea)=5:1; reaction time 1.5 h.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 4 h.The crude product was purified by column chromatography with 83.7% isolated yield.The molecular structures of all the products were characterized by 1H NMR,13C NMR and IR spectroscopy respectively.

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备注/Memo

备注/Memo:
作者简介:徐崇福(1955-),男,宁夏平罗县人,教授,主要从事药物中间体合成研究。
更新日期/Last Update: 2014-04-20