HRID216313

反应详情

EQUATION

反应方程式

HRID 216313 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

Hydrazine hydrate (30 mL) was added to a solution of (2-methyl-1-trityl-1H-imidazol-4-yl)[1-(trifluoromethyl)cyclopropyl]methanone (15.78 g, 34.2 mmol) and powdered potassium hydroxide (9.6 g, 171 mmol) in ethylene glycol (200 mL). After stirring at 120° C. for 20 min, the reaction mixture was heated at 180° C. for 2 h. After cooling to ambient temperature, water was added and the mixture was extracted twice with ethyl acetate. The combined organic extracts were washed with brine, dried (sodium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-60% ethyl acetate/hexane afforded the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated at 180° C. for 2 h
  2. temperatureAfter cooling to ambient temperature
  3. extractionthe mixture was extracted twice with ethyl acetate
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (sodium sulfate)
  6. concentrationconcentrated in vacuo