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 almotriptan midboby 4 -(pyrrolidine - 1 - sulfonylmethyl) phenylhydrazine hydrochloride was prepared from 4 - nitrophenylmethane sulfonylchloride by pyrrolidine replacement,hydrazine hydrate catalytic reduction,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% .%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%。
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