反应详情

6-Chlorohexanesulfonyl chloride (6.57g, 30 mmol) was added dropwise to a solution of diethyl ether (60 ml) and a 12% acetonitrile solution of dimethylamine (24.8 g, 66 mmol) with stirring under ice-cooling. Thereafter, the mixture was stirred at the same temperature for 20 minutes. The reaction mixture was concentrated in vacuo. Thereafter, the concentrate was diluted with diethyl ether (60 ml). The resulting solution was washed twice with water (10 ml) and then with brine (10 ml), and thereafter dried over anhydrous magnesium sulfate. Subsequently, the solvent was removed by evaporation in vacuo. The crude product was purified by column chromatography on silica gel with ethyl acetate-n-hexane (1:4), to give N,N-dimethyl-6-chlorohexanesulfonamide (6.59 g) as a pale yellow oil.

1. temperaturecooling
2. concentrationThe reaction mixture was concentrated in vacuo
3. additionThereafter, the concentrate was diluted with diethyl ether (60 ml)
4. washThe resulting solution was washed twice with water (10 ml)
5. dry with materialwith brine (10 ml), and thereafter dried over anhydrous magnesium sulfate
6. customSubsequently, the solvent was removed by evaporation in vacuo
7. customThe crude product was purified by column chromatography on silica gel with ethyl acetate-n-hexane (1:4)