反应详情

To a mixture of compound 50 (1.0 g, 2.96 mmol) and NH4Cl (46 mg, 0.86 mmol) in EtOH (29 mL)/water (15 mL) at 100° C., Fe (1.4 g, 25.15 mmol) was added in one portion and the mixture was refluxed with vigorous stirring for 40 min. The mixture was filtered through Celite®, the Celite® washed with EtOH and the combined filtrate concentrated under reduced pressure. The residue was suspended in EtOAc, washed with water; the organic phase was dried over anhydrous Na2SO4 and evaporated affording title compound 225 (916.15 mg, 91% yield). MS (m/z): 338.9 (96%), 340.9 (100%).

1. temperaturethe mixture was refluxed
2. filtrationThe mixture was filtered through Celite®
3. washthe Celite® washed with EtOH
4. concentrationthe combined filtrate concentrated under reduced pressure
5. washwashed with water
6. dry with materialthe organic phase was dried over anhydrous Na2SO4
7. customevaporated