HRID2302142

反应详情

EQUATION

反应方程式

HRID 2302142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

At 0° C., a solution of 13 g of sodium hydroxide in 80 ml of water was added to 16 g of 5-acetyloxy-2,3-dichloropyridine in 100 ml of ice-water. The mixture was subsequently initially stirred at 0° C. for one hour and then at approximately 20° C. for 17 hours, and the reaction mixture was then washed with 150 ml of ethyl acetate. The mixture was acidified up to a pH of 4-5 by addition of acetic acid and then extracted three times with 100 ml of ethyl acetate each time. The combined organic phases were dried over magnesium sulfate and finally concentrated. Yield: 12.2 g.

WORKUP

后处理

  1. waitat approximately 20° C. for 17 hours
  2. washthe reaction mixture was then washed with 150 ml of ethyl acetate
  3. additionThe mixture was acidified up to a pH of 4-5 by addition of acetic acid
  4. extractionextracted three times with 100 ml of ethyl acetate each time
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. concentrationfinally concentrated