Abstract: 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<SUB<2</SUB<SO<SUB<3</SUB<, with a yield of 96%. p-Nitrophenyl methanesulfonyl chloride（Ⅳ）, was obtained by chlorination of Ⅲ with PCl<SUB<5</SUB<, 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.