3-Nitrobenzenesulfonyl chloride → HCID 54066048, compound

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Reaction Steps

221.5 g of 3-nitro-benzenesulphonyl chloride are introduced in portions into a solution of 150 g of sulphuric acid mono-2-amino-ethyl ester and 0.6 liter of water at 60°-70° C. During this procedure, the pH value is continuously kept between 9.0 and 10.0 by adding 45% strength sodium hydroxide solution dropwise. The mixture is subsequently stirred at 60°-70° C. and pH 9.0 to 10.0 for 1 hour and then allowed to cool and the resulting precipitate is filtered off. The precipitate is washed with water and dried at 80° C. 305 g of sulphuric acid mono-N-(3-nitro-benzenesulphonyl)-2-amino-ethyl ester are obtained. This ester is dissolved in 1.5 liters of dimethylformamide and hydrogenated over Raney nickel. After subsequently filtering off the catalyst and distilling off the solvent in vacuo, about 220 g of sulphuric acid mono-N-(3-aminophenylsulphonyl)-2-aminoethyl ester are obtained. ##STR16##

Provenance & Evidence