HRID918375

反应详情

EQUATION

反应方程式

HRID 918375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 35 g of tetrahydropyran-2-yloxy acetonitrile in 100 ml of ether is added dropwise to a slurry of 10 g of lithium aluminum hydride in 300 ml of ether and 100 ml of tetrahydrofuran. The slurry is refluxed for 210 minutes, cooled, and 25 ml of sat. potassium carbonate solution is added at a rate that maintains gentle reflux. After 90 minutes the slurry is filtered and the solid is washed with ether. The filtrate is evaporated in vacuo and distilled to give 33.6 g of 2-(tetrahydropyran-2-yloxy)ethylamine, boiling point 41.5°-46°C at 0.5-0.8 mm.

WORKUP

后处理

  1. temperatureThe slurry is refluxed for 210 minutes
  2. temperaturecooled
  3. filtrationAfter 90 minutes the slurry is filtered
  4. washthe solid is washed with ether
  5. customThe filtrate is evaporated in vacuo
  6. distillationdistilled