HRID77820

反应详情

EQUATION

反应方程式

HRID 77820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (6-methyl-pyridin-2-yl)-methanol (1.44 g, 11.7 mmol), thionyl chloride (1.45 mL, 19.9 mmol) and methylene chloride (20 mL) was stirred under reflux for 40 minutes. The reaction solution was cooled to room temperature and then concentrated under a reduced pressure. The residue was partitioned into sodium bicarbonate solution and diethyl ether. The organic layer was concentrated under a reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (1.42 g, 85.8%).

WORKUP

后处理

  1. temperatureunder reflux for 40 minutes
  2. concentrationconcentrated under a reduced pressure
  3. customThe residue was partitioned into sodium bicarbonate solution and diethyl ether
  4. concentrationThe organic layer was concentrated under a reduced pressure
  5. customthe residue was purified by silica gel chromatography (ethyl acetate)