反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAfter complete addition the reaction
- temperatureThe reaction was cooled to 0° C.
- filtrationwas filtered through Celite
- washthe filter cake washed with THF and Et2O
- dry with materialThe organic filtrate was dried with anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo