反应详情

To a solution of (3-methyl-4-nitrophenyl)methanol (1.0 equiv.) in dichloromethane, pyridinium chlorochromate (1.1 equiv.) was added and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was filtered through celite and the filtrate was evaporated. The residue was adsorbed on silica (100-200 mesh) and purified by flash chromatography on silica gel, eluting with 5% ethyl acetate in petroleum ether (60-80), to provide the title compound in the form of creamish crystals (93%); 1H NMR (300 MHz, CDCl3) δ: 2.66 (s, 3H), 7.84-7.87 (m, 2H), 8.04-8.07 (d, J=8.7 Hz, 1H), 10.12 (s, 1H); IR (KBr) 3104, 3079, 2981, 2857, 2743, 1702, 1607, 1518, 1383, 1361, 1308, 1226, 1153, 1008, 832, 735 cm−1.

1. filtrationThe reaction mixture was filtered through celite
2. customthe filtrate was evaporated
3. custompurified by flash chromatography on silica gel
4. washeluting with 5% ethyl acetate in petroleum ether (60-80)