4-氨基-N-[3-(2-羟乙基)砜硫酸酯]苯基苯甲酰胺的合成

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。

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

4-Amino-N-3-(2-hydroxyethyl)sulfonylsulfatide]phenylbenzamide was synthesized using 4-nitro-N-3-(2-hydroxyethyl)sulfonyl]phenylbenzamide and chlorosulfonic 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 1H NMR.