HRID868339

反应详情

EQUATION

反应方程式

HRID 868339 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

To a stirred suspension of 11.4 g of lithium aluminum hydride in 500 ml of dry diethyl ether, 32.7 g of ethyl 6-methylnicotinate in 250 ml of dry diethyl ether is added dropwise at room temperature, and the mixture is refluxed for 1.5 hours. The reaction mixture is cooled to 0° C., and the remaining lithium aluminum hydride is decomposed by the cautious addition of 60 ml of water. The ether layer is decanted, and the residual solid is extracted with three 150-ml portions of diethyl ether. The combined extracts are dried over potassium carbonate and concentrated to give 19.6 g of crude 5-hydroxymethyl-2-methylpyridine.

WORKUP

后处理

  1. additionis added dropwise at room temperature
  2. temperaturethe mixture is refluxed for 1.5 hours
  3. customThe ether layer is decanted
  4. extractionthe residual solid is extracted with three 150-ml portions of diethyl ether
  5. dry with materialThe combined extracts are dried over potassium carbonate
  6. concentrationconcentrated