反应详情

温度

120 °C

To a solution of 4-(1H-imidazol-4-yl)-3-phenyl-5-trifluoromethyl-isoxazole (70 mg, 0.25 mmol) in DMF (2.5 mL) was added 4-fluoroacetophenone (35 mg, 0.25 mmol) and potassium carbonate (69.1 mg, 0.5 mmol) and the resulting mixture heated at 120° C. overnight. The resulting mixture was then poured into HCl (1 N, 200 mL) and extracted with ethyl acetate which was then washed with brine, dried over sodium sulphate and evaporated. Purification by preparative HPLC on reversed phase eluting with an acetonitrile/water [0.1% aq NH3 (25%)] gradient afforded the title compound (25 mg, 25%) which was obtained as a white solid. MS: m/e=398.1 [M+H]+.

1. extractionextracted with ethyl acetate which
2. washwas then washed with brine
3. dry with materialdried over sodium sulphate
4. customevaporated
5. customPurification by preparative HPLC on reversed phase
6. washeluting with an acetonitrile/water [0.1% aq NH3 (25%)] gradient