HRID2262532

反应详情

EQUATION

反应方程式

HRID 2262532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 4-(1H-imidazol-4-yl)-3-phenyl-5-trifluoromethyl-isoxazole (69.8 mg, 0.25 mmol) in DMF (1.0 mL) was added 4-fluorobenzotrifluoride (32 μL, 41 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 water and extracted with ethyl acetate which was then washed with brine, dried over sodium sulphate and evaporated. Purification by chromatography (SiO2, heptane:ethyl acetate=60:40) afforded the title compound (68 mg, 64%) which was obtained as an off-white solid. MS: m/e=424.3 [M+H]+.

WORKUP

后处理

  1. extractionextracted with ethyl acetate which
  2. washwas then washed with brine
  3. dry with materialdried over sodium sulphate
  4. customevaporated
  5. customPurification by chromatography (SiO2, heptane:ethyl acetate=60:40)