对-(二(2-氯乙基))胺基苯甲醛改进的一步合成法

Improvement on One-step Synthesis of p-(Bis(2-chloroethyl) aminobenzaldehyde

报道了由N,N-二羟乙基苯胺一步法合成对-(二(2-氯乙基))胺基苯甲醛.DMF与POCl3于0℃下搅拌反应45min,再于0℃下一次性加入N,N-二羟乙基苯胺的DMF溶液并搅拌,慢慢升温至110℃,继续反应2h得到标题化合物.反应物料比分别是:n(N,N-二羟乙基苯胺)∶n(POCl3)=1∶3.3,mt(总的DMF)∶m(N,N-二羟乙基苯胺)=4∶1,m1(POCl3加入前烧瓶中的DMF)∶m2(溶解N,N-二羟乙基苯胺的DMF)=3∶1.对-(二(2-氯乙基))胺基苯甲醛的产率为95.6%.

That N,N-Bis-hydroxyethylaniline was conveted to p-（Bis（2-chloroethyl）aminobenzaldehyde by onestage process is reported in this paper. DMF and POCI3 were stirred to react successively at 0℃ for 45 rain, subsequently,a solution of N,N-Bis-hydroxyethylaniline and DMF was rapidly added to the stirred reactive mixture at 0℃ ,and the whole reactive mixture was heated gradually to 110℃ to continue for 2h, and thus the topic compound was obtained. Reactive materials rates were as foUows：n（N,N-Bis-hydroxyethylaniline） ： n（POCI3） = 1：3.3, rot（total DMF）： m （ N, N - Bis - hydroxyethylaniline） = 4：1, m, （ DMF in flask before addition of POCI3 ） ： m2 （ DMF dissolving N, N - Bis - hydroxyethylaniline ） = 3：1. The yield of p- （Bis（2- chloroethyl）aminobenzaldehyde was 95.6%.