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
- 70 °C
PROCEDURE
实验过程
2-Phenylbenzofuran-7-carboxylic acid (40 g) is dissolved in tetrahydrofuran (300 ml) and the solution is added dropwise to a suspension of lithium aluminum hydride (19.12 g) in tetrahydrofuran (130 ml) under ice-cooling. After the mixture is stirred at 70° C. for 2 hours, water is added to the mixture to decompose excess lithium aluminum hydride and its complex. Insoluble materials are filtered off, and the filtrate is concentrated under reduced pressure to remove solvent. The residue is dissolved in ethyl acetate, and the solution is washed with water, dried and concentrated under reduced pressure to remove solvent. The residue is recrystallized from a mixture of ethyl acetate and n-hexane, whereby 7-hydroxymethyl-2-phenylbenzofuran (34.4 g) is obtained. Yield: 91%.
WORKUP
后处理
- temperaturecooling
- filtrationInsoluble materials are filtered off
- concentrationthe filtrate is concentrated under reduced pressure
- customto remove solvent
- dissolutionThe residue is dissolved in ethyl acetate
- washthe solution is washed with water
- customdried
- concentrationconcentrated under reduced pressure
- customto remove solvent
- customThe residue is recrystallized from a mixture of ethyl acetate and n-hexane