反应详情

温度

0 °C

p-Tolylsulfonyl chloride (38.8 g, 204 mmol) was added to a solution of compound 6 (31 g) in dry pyridine (200 mL) cooled to 0° C. After 1 h stirring at 0° C. the mixture was stirred at room temperature (rt) for additional 24 h and evaporated in vacuo. The syrupy residue was chromatographed on a column of silica gel (1000 mL) in system toluene-ethyl acetate (5:1). After removal of rests of p-tolylsulfonyl chloride (RF 0.9) the compound 7 was eluted with system toluene-ethyl acetate (1:2), (RF 0.5). Product containing fractions were evaporated to give 18.7 g (77%) of 7 as a colorless syrup.

1. stirringwas stirred at room temperature (rt) for additional 24 h
2. customevaporated in vacuo
3. customThe syrupy residue was chromatographed on a column of silica gel (1000 mL) in system toluene-ethyl acetate (5:1)
4. customAfter removal
5. washwas eluted with system toluene-ethyl acetate (1:2), (RF 0.5)
6. additionProduct containing fractions
7. customwere evaporated