HRID1019501

反应详情

EQUATION

反应方程式

HRID 1019501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Catechol (13.2 g, 0.12 mol) and potassium carbonate (16.6 g, 0.12 mol) were stirred in DMF (250 mL) and (2R)-glycidyl tosylate (22.8 g, 0.10 mol) was added and the reaction was stirred at 60° C. for 24 h. The reaction was cooled to room temperature and diluted with ice water (1 L) and extracted with diethyl ether (4 times). The combined organic solution was washed 3 times with 10% potassium carbonate, once with water, once with brine and evaporated in vacuo to yield a white solid which was purified by flash column chromatography (DCM:Methanol—50:1) to yield ((2S)-2,3-dihydro-benzo[1,4]dioxin-2-yl)-methanol as a solid.

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. extractionextracted with diethyl ether (4 times)
  3. washThe combined organic solution was washed 3 times with 10% potassium carbonate
  4. customonce with water, once with brine and evaporated in vacuo
  5. customto yield a white solid which
  6. customwas purified by flash column chromatography (DCM:Methanol—50:1)