反应详情

温度

0 °C

The alcohol from Example 1 (33.1 g) and 20 ml of triethylamine were dissolved in 350 ml of dichloromethane, cooled to 0° C., and treated with 11 ml methanesulfonyl chloride. After being stirred at room temperature for about 20 hours, the reaction mixture was diluted with dichloromethane (100 ml) and the organic layer was washed with three 50-ml portions of water and one of brine. Drying and concentration in vacuo gave the crude product which gradually crystallized upon standing. The solid was washed with diethyl ether, filtered, and dried to yield 12.0 g of 2-[2-(methylsulfonyloxy)ethyl]-N-(1,1-dimethylethyl)benzenesulfonamide as a white powder; m.p. 106°-108° C.

1. washthe organic layer was washed with three 50-ml portions of water and one of brine
2. customDrying
3. concentrationconcentration in vacuo
4. customgave the crude product which
5. customgradually crystallized
6. washThe solid was washed with diethyl ether
7. filtrationfiltered
8. customdried