HRID2200570

反应详情

EQUATION

反应方程式

HRID 2200570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of methyl 2-(2-ethyl-1,3-dioxolan-2-yl)acetate (1 g, 5.75 mmol) in anhydrous THF (40 mL) was added LAH (900 mg, 23.7 mmol) at 0° C. under nitrogen atmosphere, the resulting mixture was stirred at 90° C. overnight. The mixture was cooled to room temperature, and ethyl acetate was added to the mixture. The resulting slurry was filtered and the filtrate was concentrated to dryness. The crude product was purified by silica gel chromatography eluting with DCM/methanol (100:1 to 20:1) to give 2-(2-ethyl-1,3-dioxolan-2-yl)ethanol (233 mg, 27.4%) as yellow oil that was used without purification.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationThe resulting slurry was filtered
  3. concentrationthe filtrate was concentrated to dryness
  4. customThe crude product was purified by silica gel chromatography
  5. washeluting with DCM/methanol (100:1 to 20:1)