反应详情

110.7 g (0.5 mol) of 2-chloro-5-nitrobenzenesulfinic acid were dissolved in 500 ml of water at pH 6.5 and the solution was added to a solution of 65.5 g (0.55 mol) of 3-bromoprop-1-yne and 100 ml of THF. The reaction mixture was then heated to 40°-50° C. After the reaction had ended (check by TLC), the reaction product was extracted with 1.5 l of ethyl acetate, and the organic phase was neutralized and dried over sodium sulfate. The solvent was evaporated off to leave 95 g of 2-chloro-5-nitro-1-(prop-1-yn-3-ylsulfonyl)benzene (melting point 238°-241° C.). ##STR28##

1. temperatureThe reaction mixture was then heated to 40°-50° C
2. extractionthe reaction product was extracted with 1.5 l of ethyl acetate
3. dry with materialdried over sodium sulfate
4. customThe solvent was evaporated off