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三光气合成N-硝基-N,N'-二苯基脲的“一锅法”工艺
引用本文:许洪涛,申晓霞,曹丹,李雪刚,陈长水.三光气合成N-硝基-N,N'-二苯基脲的“一锅法”工艺[J].精细化工中间体,2008,38(2):27-29.
作者姓名:许洪涛  申晓霞  曹丹  李雪刚  陈长水
作者单位:华中农业大学,理学院,湖北,武汉,430070
摘    要:以N-硝基-2,4,6-三氯苯胺为原料,三光气为酰化剂,一锅法合成N-硝基-N-(2,4,6-三氯苯基)-N′-3,5-二甲基苯基脲。并确定酰化反应的优惠条件为:甲苯作溶剂、三乙胺为催化剂、n(三光气)∶n(N-硝基-2,4,6-三氯苯胺,5)=0.36∶1,反相滴加,反应温度为20℃,反应时间2h,此条件下收率为80%左右。通过元素分析、红外光谱分析、核磁氢谱对产品进行了结构鉴定。

关 键 词:“一锅法”  三光气  N-硝基-N  N′-二苯基脲
文章编号:1009-9212(2008)02-0027-03
修稿时间:2008年3月9日

The Synthesis of N-Nitro-N,N'-diphenyl Urea by One Pot Way Used Triphosgene as Acylating Agent
XU Hong-tao,SHEN Xiao-xia,CAO Dan,LI Xue-gang,CHEN Chang-shui.The Synthesis of N-Nitro-N,N'-diphenyl Urea by One Pot Way Used Triphosgene as Acylating Agent[J].Fine Chemical Intermediates,2008,38(2):27-29.
Authors:XU Hong-tao  SHEN Xiao-xia  CAO Dan  LI Xue-gang  CHEN Chang-shui
Abstract:The N'-(3,5-dimethylphenyl)-N-nitro-N-(2,4,6-trichlorophenyl)urea were obtained by one pot way based on N-nitro-2,4,6-trichloroaniline used triphosgene as acylating agent.The synthesis technological conditions were discussed. The optimum reaction conditions were obtained as follows:touluene as solvent,triethylamine as catalyst,n(triphosgene)∶n(5)= 0.36 ∶ 1,RP-dropping,temperature was 20℃,reaction time was 2 h,the yield was 80%. And the structures of the products were identified by elementary analysis,infra-red spectrum and nuclear magnetic resonance.
Keywords:one pot way  triphosgene  N-nitro-N  N'-diphenyl urea
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