反应详情

A solution of 32.5 g of the alcohol from Example 1 and 32.5 g triphenylphosphine in 244 ml of carbon tetrachloride was stirred at room temperature and under an atmosphere of nitrogen for 72 hours. Excess carbon tetrachloride was removed in vacuo to give 83 g of a crude yellow oil. Purification by silica gel chromatography (hexanes-20% ethyl acetate) afforded a colorless viscous oil which crystallized on standing. The product was isolated by trituration with hexanes, filtration, and drying. The yield of pure 2-(2-chloroethyl)-N-(1,1-dimethylethyl)benzenesulfonamide, m.p. 64°-65° C., was 15.9 g.

1. customExcess carbon tetrachloride was removed in vacuo
2. customto give 83 g of a crude yellow oil
3. customPurification by silica gel chromatography (hexanes-20% ethyl acetate)
4. customafforded a colorless viscous oil which
5. customcrystallized
6. customThe product was isolated by trituration with hexanes, filtration
7. customdrying