反应详情

To the compound 101 (2.76 g) in an ethyl acetate (32 ml) and acetic acid (16 ml) suspension, zinc powder (2.88 g) was added under ice cooling, and the mixture was stirred at that temperature for 20 minutes and at room temperature for 4 hours. The reaction mixture was filtered by a glass filter spread with Celite®, then the residue was washed with ethyl acetate (50 ml). The filtrate and the washings were combined, then the mixture was successively washed with saturated aqueous ammonium chloride solution and brine, dried over sodium sulfate, then concentrated. The residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate/methanol=6/6/1) to obtain the title compound (2.5 g).

1. filtrationThe reaction mixture was filtered by a glass
2. filtrationfilter
3. washthe residue was washed with ethyl acetate (50 ml)
4. washthe mixture was successively washed with saturated aqueous ammonium chloride solution and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate/methanol=6/6/1)