反应详情

温度

115 °C

A solution of 6-tert-butyl-2-(2-trifluoromethyl-phenyl)-3H-pyrimidin-4-one (0.47 g, 1.59 mmol) in phosphorous oxychloride (1.65 mL, 15.9 mmol) was treated with tri-n-propylamine (0.61 mL, 3.17 mmol) and heated at 110-120° C. for 1 hour. The solvent was removed by evaporattion then azeotroped three times with toluene. 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 (0.33 g, 66% yield) as a yellow oil. 1H NMR (CDCl3, 500 MHz) δ 1.31 (9H, s), 7.25 (s, 1H), 7.51 (t, J=7.6 Hz, 1H), 7.58 (t, J=7.5 Hz, 1H), 7.74 (t, J=8.5 Hz, 2H) ppm; MS (FIA) 314.9 (M+H); Rt (Method A) 4.156 minutes.

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