HRID1243812

反应详情

EQUATION

反应方程式

HRID 1243812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-bromo-6-cyano-3-methylpyridine (272 mg) and benzyl alcohol (156 mg) in tetrahydrofuran (20 mL) was added sodium hydride (40 mg), and the mixture was heated under reflux for one hour. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed successively with saturated aqueous sodium bicarbonate and saturated brine, and dried over anhydrous sodium sulfate. After removal of the sodium sulfate by filtration, the organic solvent was evaporated off in vacuo. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=19:1) to give the title compound (161 mg) as a colorless liquid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for one hour
  3. washwashed successively with saturated aqueous sodium bicarbonate and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customAfter removal of the sodium sulfate
  6. filtrationby filtration
  7. customthe organic solvent was evaporated off in vacuo
  8. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=19:1)