HRID1515733

反应详情

EQUATION

反应方程式

HRID 1515733 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 solution of (tetrahydro-pyran-2-yl)-acetic acid ethyl ester (77.1 g, 0.45 mol) in tetrahydrofuran (1.5 L) at 0° C. was added lithium aluminium hydride (22.1 g, 0.58 mol) in several portions. The mixture was stirred at 0° C. for 2 h and quenched with 1 N sodium hydroxide solution. The mixture was filtered and the filter cake was washed with dichloromethane (4×300 mL). The combined organic layers were concentrated in vacuo. The crude product was purified by distillation under reduced pressure to afford 2-(tetrahydro-pyran-2-yl)-ethanol (53.5 g, 92% yield) as a colorless oil.

WORKUP

后处理

  1. customquenched with 1 N sodium hydroxide solution
  2. filtrationThe mixture was filtered
  3. washthe filter cake was washed with dichloromethane (4×300 mL)
  4. concentrationThe combined organic layers were concentrated in vacuo
  5. distillationThe crude product was purified by distillation under reduced pressure