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| 有机锡催化苯氨基甲酸甲酯分解的研究 | |
| 引用本文： | 戴云生,王越,姚洁,王庆印,刘良明,崔黎黎,赵永峰,王公应.有机锡催化苯氨基甲酸甲酯分解的研究[J].化学学报,2007,65(11):1064-1070. |
| 作者姓名： | 戴云生 王越 姚洁 王庆印 刘良明 崔黎黎 赵永峰 王公应 |
| 作者单位： | 1. 中国科学院成都有机化学研究所,成都,610041;中国科学院研究生院,北京,100039 2. 中国科学院成都有机化学研究所,成都,610041 3. 胜利油田胜利化工有限公司,东营,257503 |
| 摘 要： | 对几种锡化合物催化苯氨基甲酸甲酯(MPC)热分解制苯基异氰酸酯(PI)反应进行了研究, 发现二丁基氧化锡具有较高的催化活性. 用HPLC-MS确定了分解的未知副产物为二苯基碳化二亚胺(DPCD). 分析认为生成N,N'-二苯基脲(DPU)和DPCD的反应为合成PI的主要竞争反应. 常压下以Bu2SnO为催化剂时的适宜反应条件为以邻二氯苯(ODCB)为溶剂, 溶剂用量为MPC用量的15倍(质量比), Bu2SnO用量为MPC用量的0.075 (摩尔比), 反应时间1 h. 此条件下MPC转化率为85.17%, PI收率为67.65%. |
| 关 键 词： | 苯氨基甲酸甲酯 苯基异氰酸酯 催化分解 二丁基氧化锡 |
| 收稿时间： | 2006-9-30 |
| 修稿时间： | 2006-09-302006-12-18 |
Study on Organotin-catalyzed Decomposition of Methyl N-phenyl Carbamate |
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| DAI,Yun-Sheng,WANG,Yue,YAO,Jie,WANG,Qing-Yin,LIU,Liang-Ming,CUI,Li-Li,ZHAO,Yong-Feng,WANG,Gong-Ying.Study on Organotin-catalyzed Decomposition of Methyl N-phenyl Carbamate[J].Acta Chimica Sinica,2007,65(11):1064-1070. | |
| Authors: | DAI Yun-Sheng WANG Yue YAO Jie WANG Qing-Yin LIU Liang-Ming CUI Li-Li ZHAO Yong-Feng WANG Gong-Ying |
| Institution: | 1. Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041;2.Graduate School of the Chinese Academy of Sciences, Beijing 100039;3. Shengli Chemical Company Limited of Shengli Oil Field, Dongying 257503 |
| Abstract: | The synthesis of phenyl isocyanate (PI) was studied by thermal decomposition of methyl N-phenyl carbamate (MPC) over tin catalysts. It has been found that di-n-butyltin oxide had higher activity. The unknown byproduct was determined as diphenylcarbodiimide (DPCD) by HPLC-MS. The results show that the formation of N,N'-diphenylurea (DPU) and DPCD are the main competitive reactions to the synthe-sis of PI. At normal pressure,the conversion of MPC is 85.17% and the yield of PI is 67.65% over Bu2SnO under the optimal reaction condition,which is as follows: solvent,o-dichlorobenzene (ODCB); m(ODCB)/m(MPC)=15; n(Bu2SnO)/n(MPC)=0.075; reaction time,1 h. |
| Keywords: | methyl N-phenyl carbamate phenyl isocyanate catalytic decomposition di-n-butyltin oxide |
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