HRID931034

反应详情

EQUATION

反应方程式

HRID 931034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of 3-oxa-8-azabicyclo[3.2.1]octan-8-yl(8-bromo-6-(trifluoromethyl)imidazo[1,2-a]pyridin-3-yl)methanone (315 mg), 1H-1,2,4-triazole (108 mg), copper(I) iodide (44.5 mg), 8-quinolinol (33.9 mg) and potassium carbonate (215 mg) in DMSO (3.0 mL) was stirred with microwave irradiation at 170° C. for 30 min. To the reaction mixture was added 0.1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous ammonium chloride solution and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane), and the obtained solid was recrystallized from ethyl acetate/hexane to give the title compound (22.0 mg).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated aqueous ammonium chloride solution and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  6. customthe obtained solid was recrystallized from ethyl acetate/hexane