摘要
以对硝基氯苄为起始原料,采用一锅法经亚硫酸钠磺化、氯气氯代制得对硝基苯甲磺酸酰氯,再经四氢吡咯取代、水合肼催化还原、重氮化、保险粉还原制得阿莫曲坦中间体4-(吡咯烷-1-基磺酰甲基)苯肼盐酸盐。硝基还原采用水合肼/Fe2O3-MgO系催化剂催化还原,收率92%;用保险粉还原重氮液制备肼盐酸盐,收率69%。
With 4-nitrobenzyl chloride as the starting material,the one-pot method was adopted to prepare 4-nitrophenylmethane sul- fonylchloride by sulfonation of sodium sulfite and chlorination of chlorine; the ahnotriptan midboby 4-（pyrrolidine-1-sulfonylmethyl） phenylhydrazine hydrochloride was prepared from 4-nitrophenylmethane sulfonylchloride by pyrrolidine replacement, hydrazine hydrate catalytic reduetion,diazotization and sodium hydrosulfite reduction. Nitro reduction adopted hydrazine hydrate/Fe2O3- MgO catalyst reduction, the yield was 92% ;hydrazine hydrochloride was prepared by the reduction of diazo liquid with sodium hydrosulfite,the yield was 69%.
出处
《中国药业》
CAS
2014年第16期34-35,共2页
China Pharmaceuticals
基金
江西省科技厅科技支撑计划项目
项目编号:20133BBE50015
