第 38 卷第 2 期Vol. 38 No. 2
2008 年 4 月Apr 2008

所属栏目:农药及中间体

三光气合成N-硝基-N,N-二苯基脲的“一锅法”工艺
许洪涛,申晓霞,曹 丹,李雪刚,陈长水 (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2 h,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
中图分类号:TQ452  文献标识码:A  文章编号:1009-9212(2008)02- 0027-03
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 (College of Science,Huazhong Agriculture University,Wuhan 430070,China)
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.
Key words:one pot way;triphosgene;N-nitro-N,N'-diphenyl urea
基金项目:国家自然科学基金资助项目(39770845)。
作者简介:许洪涛(1983-),男,湖北仙桃人,硕士研究生,主要从事农药与生物活性研究。(E-mail:hongtao_xu@webmail.hzau.edu.cn)
联 系 人:陈长水(1957-),男,教授。研究方向:农药合成及生物活性研究。(E-mail:chenchang@mail.hzau.edu.cn)
收稿日期:2008-03-09