HRID337668

反应详情

EQUATION

反应方程式

HRID 337668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-bromo-2-fluoropyridine (1 eq.), benzyl alcohol (1.2 eq.) and dibenzo-18-crown-6 (0.05 eq.) in toluene (0.4 M) was added potassium hydroxide (2 eq.). A Dean-Stark apparatus was then attached and the reaction suspension was heated at reflux for 3 h. After cooling to RT, the reaction mixture was diluted with hexanes and then filtered through a pad of celite. Concentration of the filtrate in vacuo afforded a yellow oil. Purification of the crude product thus obtained by way of column chromatography (SiO2, 97:3 (v/v) Hex:Et2O) afforded the title compound as a colorless oil.

WORKUP

后处理

  1. temperaturethe reaction suspension was heated
  2. temperatureat reflux for 3 h
  3. filtrationfiltered through a pad of celite
  4. customConcentration of the filtrate in vacuo afforded a yellow oil
  5. customPurification of the crude product
  6. customthus obtained by way of column chromatography (SiO2, 97:3 (v/v) Hex:Et2O)