HRID77825
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 5 minutes
- customwas allowed to room temperature
- concentrationconcentrated under a reduced pressure
- customThe resulting residue was partitioned into diethyl ether and saturated sodium bicarbonate solution
- customThe organic layer was purified by silica gel column chromatography (ethyl acetate)