HRID385569

反应详情

EQUATION

反应方程式

HRID 385569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder cooling with ice
  2. distillationThe solvent was distilled off under reduced pressure, water
  3. additionwas added
  4. stirringthe mixture was stirred
  5. temperatureunder cooling with ice
  6. filtrationThe solid was filtered off
  7. additionchloroform was added
  8. dry with materialthe resultant was dried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure
  10. additionThereto was added diethyl ether
  11. filtrationthe solid was filtered off