HRID1482189

反应详情

EQUATION

反应方程式

HRID 1482189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

(S)-2-Hydroxy-3-phenylpropanoic acid (1.0 g, 6.02 mmol) was dissolved in THF (100 ml), sodium hydride (0.48 g, 12.00 mmol) and methyl iodide (1.71 g, 12.04 mmol) were added, and the mixture was stirred at 65° C. for one hour. After leaving to cool, the reaction solution was concentrated under reduced pressure and adjusted to pH 4 by adding a 6 M aqueous hydrochloric acid solution thereto. The aqueous layer was extracted with ethyl acetate, the organic layer was concentrated, and the resulting residue was purified by column chromatography (dichloromethane:methanol=10:1) to afford the title compound (0.71 g, 59%).

WORKUP

后处理

  1. customAfter leaving
  2. temperatureto cool
  3. concentrationthe reaction solution was concentrated under reduced pressure
  4. additionby adding a 6 M aqueous hydrochloric acid solution
  5. extractionThe aqueous layer was extracted with ethyl acetate
  6. concentrationthe organic layer was concentrated
  7. customthe resulting residue was purified by column chromatography (dichloromethane:methanol=10:1)