反应详情

1-(2,4-Dichloro-phenyl)-3-methyl-butan-1-ol (600 mg, 2.57 mmol) and Dess-Martin periodinane (1092 mg, 2.57 mmol) in DCM (25 ml) is stirred at RT for 2 hours. The reaction mixture is added to EtOAc (200 ml) and washed with sat. sodium metabisulfite (200 ml), sat. NaHCO3 (200 ml), brine, dried over MgSO4 and concentrated in vacuo. The crude product is purified using an ISCO combiflash chromatography, eluting with 0 to 100% (EtOAc/iso-hexane) on a 40 g silica-column to give 1-(2,4-Dichloro-phenyl)-3-methyl-butan-1-one as a yellow oil; 1H NMR (400 MHz, CDCl3) δ 7.45 (1H, d, J 1.9), 7.42 (1H, d, J 8.3), 7.32 (1H, dd, J 8.3, 1.9), 2.83 (2H, d, J 6.9), 2.25 (1H, sept, J 6.7), 1.00 (6H, d, J 6.7).

1. washwashed with sat. sodium metabisulfite (200 ml), sat. NaHCO3 (200 ml), brine
2. dry with materialdried over MgSO4
3. concentrationconcentrated in vacuo
4. customThe crude product is purified
5. washeluting with 0 to 100% (EtOAc/iso-hexane) on a 40 g silica-column