反应详情

To a solution of the product from Step D (2.70 g, 9.4 mmol) in dichloromethane (15 mL) was added 3-chloro-perbenzoic acid (2.31 g, 10.3 mmol, 77% pure) and the mixture stirred at ambient temperature for 1 h. Additional 3-chloro-perbenzoic (0.2 g, 0.9 mmol) was added and the reaction continued for 3 h. The reaction was quenched with saturated aqueous sodium bicarbonate (100 mL) and extracted with dichloromethane (50 mL). The extract was dried (MgSO4) and evaporated to a white solid (1.59 g, 56%): mp 110-111° C.; LC/MS (+APCI) m/z 304 (M+H).

1. additionAdditional 3-chloro-perbenzoic (0.2 g, 0.9 mmol) was added
2. waitthe reaction continued for 3 h
3. customThe reaction was quenched with saturated aqueous sodium bicarbonate (100 mL)
4. extractionextracted with dichloromethane (50 mL)
5. dry with materialThe extract was dried (MgSO4)
6. customevaporated to a white solid (1.59 g, 56%)