HRID77825

反应详情

EQUATION

反应方程式

HRID 77825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture solution of (4-methyl-pyridine-2-yl)-methanol (410 mg, 3.33 mmol) described in Manufacturing Example 11-1-3, thionyl chloride (0.49 mL, 6.66 mmol) and methylene chloride (10 mL) was stirred under reflux for 5 minutes. The reaction solution was allowed to room temperature and concentrated under a reduced pressure. The resulting residue was partitioned into diethyl ether and saturated sodium bicarbonate solution. The organic layer was purified by silica gel column chromatography (ethyl acetate) to obtain the title compound (340 mg, 72.1%).

WORKUP

后处理

  1. temperatureunder reflux for 5 minutes
  2. customwas allowed to room temperature
  3. concentrationconcentrated under a reduced pressure
  4. customThe resulting residue was partitioned into diethyl ether and saturated sodium bicarbonate solution
  5. customThe organic layer was purified by silica gel column chromatography (ethyl acetate)