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机构地区:[1]北京理工大学化工与环境学院,北京100081
出 处:《北京理工大学学报》2004年第6期552-554,共3页Transactions of Beijing Institute of Technology
摘 要:以氯苄为原料,经4步反应制得p-硝基苯甲磺酰吡咯烷.氯苄用发烟硝硫混酸硝化得p-硝基氯苄,产率为52%.p-硝基氯苄与亚硫酸钠反应得p-硝基苯甲磺酸钠,产率为96%.p-硝基苯甲磺酸钠用五氯化磷氯化得到p-硝基苯甲磺酰氯,产率为78%.p-硝基苯甲磺酰氯用吡咯烷氨解后得到目标产物,产率为98%.对各步反应的工艺进行了改进,提高了产率.1-(4-Nitrophenyl methanesulfonyl) pyrrolidine (Ⅴ) was prepared by four-step reactions, starting from benzyl chloride (Ⅰ). p-Nitro benzyl chloride(Ⅱ)was prepared by the nitration of Ⅰwith fuming nitric acid-fuming sulfuric acid, with a yield of 52%. Sodium p-nitro benzyl sulfonate (Ⅲ)was prepared by the sulfonation of Ⅱ with Na_2SO_3, with a yield of 96%. p-Nitrophenyl methanesulfonyl chloride(Ⅳ), was obtained by chlorination of Ⅲ with PCl_5, with a yield of 78%. Aminolysis of Ⅳ with pyrrolidine gave the title compound Ⅴ, with a yield of 98%. The procedure was improved and total yield was increased.
关 键 词:制备 p-硝基苯甲磺酰吡咯烷 氯苄
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