HRID385569
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
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a solution of 10 g of 5-(benzyloxy)-2-(hydroxymethyl)pyridin-4(1H)-one in 58 mL of pyridine, 4.6 mL of acetyl chloride was added under cooling with ice, and the mixture was stirred at 60 to 70° C. for 3 hours. The solvent was distilled off under reduced pressure, water was added thereto, and the mixture was stirred under cooling with ice. The solid was filtered off, chloroform was added thereto and the resultant was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. Thereto was added diethyl ether and the solid was filtered off to obtain 9.2 g of (5-(benzyloxy)-4-oxo-1,4-dihydropyridin-2-yl)methyl acetate as a light brown solid.
WORKUP
后处理
- temperatureunder cooling with ice
- distillationThe solvent was distilled off under reduced pressure, water
- additionwas added
- stirringthe mixture was stirred
- temperatureunder cooling with ice
- filtrationThe solid was filtered off
- additionchloroform was added
- dry with materialthe resultant was dried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- additionThereto was added diethyl ether
- filtrationthe solid was filtered off