反应详情

温度

85 °C

2-Methyl-4-trifluoromethoxy-benzamide 14 (2.0 g, 9.1 mmol) was taken up in phosphorus oxychloride (15 mL) and heated to 85° C. for 2 hrs. The excess phosphorus oxychloride was removed under reduced pressure and the resulting residue partitioned between sat. aqueous sodium bicarbonate and ether. The organic layer was dried (sodium sulfate) and concentrated. The residue was passed through silica gel using 25% ether/hexanes to remove trace impurities and yielded a colorless solid (90%). 1H NMR (400 MHz,CDCl3) δ7.65 (d, J=8.4 Hz. 1 H, Ar), 7.17 (s, 1 H, Ar), 7.13 (d, J=8.4 Hz, 1 H, Ar), 2.6 (s, 3 H, CH3).

1. customThe excess phosphorus oxychloride was removed under reduced pressure
2. customthe resulting residue partitioned between sat. aqueous sodium bicarbonate and ether
3. dry with materialThe organic layer was dried (sodium sulfate)
4. concentrationconcentrated
5. customto remove trace impurities