微波辐射合成N-芳基哌嗪盐酸盐

Synthesis of N-aryl piperazine hydrochloride under microwave irradiation

芳胺与N,N-双(2-氯乙基)胺盐酸盐在微波辐射下反应合成N-芳基哌嗪盐酸盐,得到一系列的重要中间体(3a～3g),所有的化合物结构经IR、1H NMR、MS表征确证。以苯基哌嗪盐酸盐的微波合成为例,考察了微波辐照时间、辐射温度、原料投料比等三个方面对苯胺转化率或主产物收率的影响。得到优化合成条件:微波辐射反应时间为20 min,微波辐射反应温度为120℃,芳胺与N,N-双(2-氯乙基)胺盐酸盐的摩尔比为1∶0.9。与传统加热方法制备N-芳基哌嗪盐酸盐相比,微波辐射下反应速度至少是常规合成方法反应速度的20倍。

N-Aryl piperazine hydrochlorides were synthesized from arylamines and N, N-bis（2-chloroeth- yl） amine hydroehloride under microwave irradiation. The compounds were characterized by IR,^1H NMR and MS. The effects of irradiation time, irradiation temperature and mole ratio on the conversion rate of aniline or the yield of 3 a were discussed. The optimum conditions were as follows ： irradiation time 20 min ; reaction temperature 120 ℃, mole ratios of aniline and N, N-bis （2-chloroethyl） amine hydrochloride 1 ： 0.9. Under microwave irradiation the reaction is 20 times faster than that under conventional conditions.