4-氨基-N-[3-(2-羟乙基)砜硫酸酯]苯基苯甲酰胺的合成

Synthesis of 4-Amino-N-[3-(2-hydroxyethyl)sulfonylsulfatide] phenylbenzamide

以4-硝基-N-[3-（2-羟乙基）砜基]苯基苯甲酰胺和氯磺酸为主要原料,经过加氢和酯化2步反应合成了4-氨基-N-[3-（2-羟乙基）砜硫酸酯]苯基苯甲酰胺。实验表明,加氢反应的较佳条件：4-硝基-N-[3-（2-羟乙基）砜基]苯基苯甲酰胺（质量,g）与甲醇（体积,mL）比1∶18,Raney-Ni催化剂质量分数40%,氢气压0.4~0.6 MPa,反应温度60℃,反应时间80 min,收率86%。酯化反应的较佳条件：n（4-氨基-N-[3-（2-羟乙基）砜基]苯基苯甲酰胺）∶n（氯磺酸）=1∶1.05,反应温度40℃,反应时间8 h,收率92%。产物及中间体的结构经过了IR1、H NMR表征,确定为目标产物。

4-Amino-N-[3-（2-hydroxyethy]） sulfonylsulfatide-] phenylbenzamide was synthesized using 4-nitro-N-V3-（2-hydroxyethyl）sulfonyl]phenylbenzamide and chlorosulfo- nic acid as starting materials through hydrogenation and esterification. The obtained optimum conditions for hydrogenation were using methanol as solvent, Raney-Ni as catalyst, temperature 60 ℃, pressure 0. 4~0. 6 MPa, reaction time 80 min. Under above conditions, the yield was 86%. The obtained optimum conditions for esterification were n （4-amino-N-[3- （2-hydroxyethyl） sulfonyl] phenylbenzamide） ： n （chlorosulfonic acid） - 1： 1.05, temperature 40℃, reaction time 8 h. Under above conditions, the yield was 92%. The obtained product and intermediate were characterized by IR and 3H NMR.