HRID963211

反应详情

EQUATION

反应方程式

HRID 963211 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

To a stirred 0° C. solution of THF (~50 mL) containing LAH (0.86 g, 22.6 mmol) under N2 atmosphere was added dropwise a THF solution of ethyl 2,3-dihydrobenzo[1,2-b]furan-3-acetate (2.50 g, 11.3 mmol). After complete addition the reaction was allowed to warm to 22° C. and stand for two h. The reaction was cooled to 0° C. and treated sequentially with water (0.9 mL), 15% NaOH (0.9 mL), and water (2.7 mL). After stirring for 2 h the reaction was filtered through Celite and the filter cake washed with THF and Et2O. The organic filtrate was dried with anhydrous MgSO4, filtered, and concentrated in vacuo to afford a the title compound (1.85 g, >99%) as a yellow oil which was used without further purification.

WORKUP

后处理

  1. additionAfter complete addition the reaction
  2. temperatureThe reaction was cooled to 0° C.
  3. filtrationwas filtered through Celite
  4. washthe filter cake washed with THF and Et2O
  5. dry with materialThe organic filtrate was dried with anhydrous MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo