反应详情

A solution of diazomethane (Diazald, 2.70 g) in MeOH (15 mL) was added dropwise to a mixture of ketone 1A (997 mg) and KOH (3.81 g) in MeOH (10 mL) and water (1.8 mL) at 0° C. over a period of 1.5 h. The reaction mixture was allowed to warm to rt and was maintained for 16 h. The resulting suspension was concentrated and was diluted with water (50 mL). The resulting aqueous suspension was extracted with ether (1×), then with DCM (2×), and the combined organic layers were dried (Na2SO4) and concentrated. The residue was purified by silica gel chromatography (0/100 to 10/90 MeOH/EtOAc) to provide 964 mg of ketone 8A as a white solid. Data: LC/MS (ESR) m/z 222 [M+1]+, 244 [M+Na]+.

1. temperaturewas maintained for 16 h
2. concentrationThe resulting suspension was concentrated
3. additionwas diluted with water (50 mL)
4. extractionThe resulting aqueous suspension was extracted with ether (1×)
5. dry with materialwith DCM (2×), and the combined organic layers were dried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by silica gel chromatography (0/100 to 10/90 MeOH/EtOAc)