反应详情

温度

115 °C

A solution of 6-methyl-2-(2-trifluoromethyl-phenyl)-3H-pyrimidin-4-one (10.7 g, 41.9 mmol) in phosphorous oxychloride (39 mL, 419 mmol) was treated with tri-n-propylamine (16 mL, 83.9 mmol) and refluxed at 110-120° C. for 1 hours. The solvent was evaporated, azeotroped three times with toluene, then dried in vacuo. The residue was taken up in ethyl acetate, washed sequentially with 1 N sodium hydroxide, water and brine, then dried over sodium sulfate and concentrated. Purification by flash chromatography [SiO2, ethyl acetate:hexanes (1:9)] provided the title compound (9.61 g, 84% yield) as an orange oil.

1. customThe solvent was evaporated
2. customazeotroped three times with toluene
3. customdried in vacuo
4. washwashed sequentially with 1 N sodium hydroxide, water and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customPurification by flash chromatography [SiO2, ethyl acetate:hexanes (1:9)]