反应详情

温度

0 °C

The product from Step B (4 g, 27.28 mmol) was dissolved in dichloromethane (100 mL) and cooled to 0° C. To this solution was added pyridinium chlorochromate (5.5 g, 25.53 mmol) and the reaction was stirred at this temperature for 1 h. The reaction mixture was washed with 1 M aqueous solution of hydrogen chloride. The organic layer was separated, dried (MgSO4), and concentrated to give an oil, which was purified by flash chromatography (silica gel, ethyl acetate/hexane: 1/9): 1H NMR (CDCl3) δ 4.15 (s, 3H, CH3), 7.61 (m, 3H, Ar—H), 7.87 (m, 2H, Ar—H), 8.28 (m, 1H, Ar—H), 10.61 (s, 1H, CHO); MS 191 (M+NH4+).

1. washThe reaction mixture was washed with 1 M aqueous solution of hydrogen chloride
2. customThe organic layer was separated
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customto give an oil, which
6. customwas purified by flash chromatography (silica gel, ethyl acetate/hexane: 1/9)