HRID964536

反应详情

EQUATION

反应方程式

HRID 964536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution prepared by dissolving 29.5 g, of 2,3-dimethoxycarbonylpyridine in 200 ml of ethylether was added dropwise to a solution prepared by suspending 10 g of lithium aluminum hydride in 300 ml of dried ethylether at 0° C. This mixed solution was stirred at 20° C. for 3 hours and 30 ml of water was slowly added thereto at 0° C. The resulting solution was stirred for 5 hours at the room temperature and solid was filtered through celite. The filtrate was evaporated under reduced pressure and then the residual product was purified by a silica gel column chromatography (chloroform : methanol (10:1)) to give 10.4 g of the above title compound (yield: 75%).

WORKUP

后处理

  1. customA solution prepared
  2. dissolutionby dissolving 29.5 g
  3. customprepared
  4. customat 0° C
  5. customat 0° C
  6. stirringThe resulting solution was stirred for 5 hours at the room temperature and solid
  7. filtrationwas filtered through celite
  8. customThe filtrate was evaporated under reduced pressure
  9. customthe residual product was purified by a silica gel column chromatography (chloroform : methanol (10:1))