N,N′-双(对甲苯磺酰基)-2-哌嗪羧酸甲酯的合成

由乙二胺和对甲苯磺酰氯反应制得N,N′-双(对甲苯磺酰基)乙二胺。此步最佳工艺条件为:n(对甲苯磺酰氯)∶n(乙二胺)=2.2∶1,反应溶剂为苯,反应温度为40～45℃,反应时间为6h,收率80%。由丙烯酸甲酯和溴反应制得α,β-二溴丙酸甲酯,收率为88%。再由上述二种中间体反应合成标题化合物,此步省略了N,N′-双(对甲苯磺酰基)乙二胺的二钠盐制备,收率为73%。

Synthesis of Methyl-N,N′-bis(p-methyl phenyl sulfonyl)-2-piperazinecarboxylate

N,N′-Bis(p-methyl phenyl sulfonyl)ethylene diamine was synthesized by reacting ethylenediamine with p-toluenesulfonylchloride. The optimum reaction conditions were as follows:molar ratio of p-toluenesulfonylchloride to ethylenediamine,2.2∶1; solvent, C_6H_6; reaction temperature,40~45℃; reaction time,6 h. The yield was 80%. Methyl-α,β-dibromo propionate was synthesized by reacting methyl acrylate with bromine with a yield of 88%. The title compound was synthesized by reacting the above products directly without the preparation of disodium salt of N,N′-bis(p-methyl phenyl sulfonyl)ethylene diamine with a yield of 73%.