盐酸催化合成二苯甲烷二氨基甲酸甲酯 |
| |
引用本文: | 谢可卫,项曙光,韩方煜.盐酸催化合成二苯甲烷二氨基甲酸甲酯[J].化工中间体,2008(7):1-3. |
| |
作者姓名: | 谢可卫 项曙光 韩方煜 |
| |
作者单位: | 青岛科技大学炼油化工高新技术研究所,山东,青岛,266042 |
| |
摘 要: | 用碳酸二甲酯(DMC)代替光气,与苯胺甲氧羰基化反应制得苯氨基甲酸甲酯(MPC),在盐酸催化剂的作用下,经甲基化缩合反应合成了4,4-二苯甲烷二氨基甲酸甲酯(MDC);使用液-质联用仪分析了反应物组成;测定了MDC的熔点;采用核磁共振仪对产品结构进行了表征;考察了反应温度、物料配比、反应时间、催化剂用量对MDC收率的影响。实验结果表明,在n(MPC/甲醛)=6:1、15%盐酸用量15mL、反应温度90℃、反应时间3h的条件下,MDC收率达到63%。该合成方法具有便于光气法改造、反应条件温和、催化剂易得易分离等优点。
|
关 键 词: | 二苯甲烷二氨基甲酸甲酯 苯氨基甲酸甲酯 甲醛 盐酸 缩合反应 |
Synthesis of Methylene Diphenyl Dicarbamate Catalyzed by Hydrochloric Acid |
| |
Authors: | XIE Ke-wei XIANG Shu-guang HAN Fang-yu |
| |
Affiliation: | (Hi-Tecb Institute for Petroleum and Chemical Industry, Qingdao University of Science and Technology, Qingdao 266042,Sbandong, China) |
| |
Abstract: | Using dimethyl carbonate (DMC) to replace phosgene, and aniline methoxy carbonylation reaction in the benzene methyl carbamate (MPC), the role of a catalyst in hydrochloric acid, and the condensation reaction of methyl 4,4'-diphenylmethane dicarbamate (MDC), the use of liquid-mass spectrometry analysis of the response of the instrument was composed of the melting point of the MDC; using NMR structure of the products were characterized; investigated the reaction temperature, the material ratio, reaction time, the amount of catalyst on the yield of the MDC. The experimental results show that:n (MPC/HCHO)=6:1, 15%hydrochloric acid 15mL, reaction temperature 90℃, and time 3h, yield of MDC can reach 63%.The practical method has advantages : facilitate the transformation of phosgene, mild reaction conditions, the catalyst easy to get and separation. |
| |
Keywords: | methylene diphenyl dicarbamate methyl N-phenyl carbamate formaldehyde hydrochlo- ric acid condensation reaction |
本文献已被 维普 万方数据 等数据库收录! |
|