反应详情

Benzoylchloride (600 mg, 4.2 mmol) was added to a solution of 20 (450 mg, 1.87 mmol) in dry pyridine (50 ml) and the reaction was allowed to proceed at 25° C. with stirring for 48 h. The reaction mixture was poured onto ice water (50 ml) and extracted with dichloromethane (3×50 ml). The dichloromethane extract was dried over sodium sulfate, the solvent was removed in vacuo and the residue obtained was purified by elution from a silica gel column using chloroform-methanol (97:3, v/v) as eluent to yield 22 as a viscous oil (550 mg, 65.4%) which was used directly in the next reaction step.

1. customto proceed at 25° C.
2. additionThe reaction mixture was poured onto ice water (50 ml)
3. extractionextracted with dichloromethane (3×50 ml)
4. extractionThe dichloromethane extract
5. dry with materialwas dried over sodium sulfate
6. customthe solvent was removed in vacuo
7. customthe residue obtained
8. customwas purified by elution from a silica gel column