反应详情

Dimethylsulfamoyl chloride (0.72 g, 0.54 ml, 0.005 mol) is added dropwise to a solution of 2.00 g (0.005 mol) of 4-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine and 2 ml of triethylamine in 20 ml of dimethylformamide. The reaction is stirred for 19 hours and then partitioned with chloroform-aqueous sodium carbonate. The organic phase is dried over anhydrous sodium sulfate, concentrated, and chromatographed with methylene chloride to 1% methanol/chloroform on silica gel to give 2.24 g of 1-[(dimethylamino)sulfonyl]-4-[4-[[7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine. This is crystallized from methylene chloride-cyclohexane to give 1.60 g of 1-[(dimethylamino)sulfonyl]-4-[4-[[-7-(trifluoromethyl)-4-quinolinyl]amino]benzoyl]piperazine of melting point 223°-224.5° C.

1. custompartitioned with chloroform-aqueous sodium carbonate
2. dry with materialThe organic phase is dried over anhydrous sodium sulfate
3. concentrationconcentrated
4. customchromatographed with methylene chloride to 1% methanol/chloroform on silica gel