反应详情

To a stirred solution of Compound 26 (660 mg, 1.25 mmol) in ethyl acetate (6 ml) was added c. HCl aq. (2 ml) with ice-cooling. The reaction mixture was stirred at room temperature for 50 min. The mixture was basified to pH10-11 with 10% NaOH aq. with ice-cooling. The organic layer was separated and the aqueous layer was extracted with AcOEt. The combined solution was washed with brine, dried (MgSO4), and concentrated in vacuo to give crude product as a pale yellow oil. The crude product was purified by column chromatography on silica gel with dichloromethane-methanol (20:1) to give Compound 27 (360 mg, 70%) as a yellow oil.

1. temperaturecooling
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with AcOEt
4. washThe combined solution was washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto give crude product as a pale yellow oil
8. customThe crude product was purified by column chromatography on silica gel with dichloromethane-methanol (20:1)