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作 者:许洪涛[1] 申晓霞[1] 曹丹[1] 李雪刚[1] 陈长水[1]
出 处:《精细化工中间体》2008年第2期27-29,共3页Fine Chemical Intermediates
基 金:国家自然科学基金资助项目(39770845)
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。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.
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