HRID385865

反应详情

EQUATION

反应方程式

HRID 385865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of NaH (64 mg, 1.59 mmol) in THF (4 mL) at 0° C. under argon was added 5-(chloromethyl)-1,3-dimethyl-1H-pyrazole (230 mg, 1.59 mmol) and allowed to stir for 20 minutes. (6-Bromopyridin-2-yl)methanol (150 mg, 0.80 mmol) was then added and the mixture was allowed to warm to room temperature and then heated to 55° C. overnight. The reaction was then cooled to ambient temperature and quenched by the addition of water. The quenched reaction mixture was diluted with water (10 mL) and DCM (10 mL) and shaken. The suspensions were passed through disposable phase separators and the DCM eluent was captured and evaporated to dryness to afford the title compound which was used without further purification.

WORKUP

后处理

  1. temperatureheated to 55° C. overnight
  2. temperatureThe reaction was then cooled to ambient temperature
  3. customquenched by the addition of water
  4. customThe quenched reaction mixture
  5. stirringshaken
  6. customevaporated to dryness