HRID1094448
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
- 0 °C
PROCEDURE
实验过程
To a 1M solution of lithium aluminum hydride in THF (57 mL) at 0° C. is added a solution of 2-fluoro-5-methylbenzoic acid (8.0 g, 52 mmol) in 160 mL of ether drop-wise. The reaction is then heated at reflux for 1.5 hr. The reaction is then cooled to 0° C. and is quenched with H2O (4 mL), aqueous 40% NaOH (4 mL) and H2O (4 mL). The resultant slurry is then filtered through celite and MgSO4. The filtrate is then concentrated and purified by silica gel flash column chromatography to provide the title compound.
WORKUP
后处理
- temperatureThe reaction is then heated
- temperatureat reflux for 1.5 hr
- customis quenched with H2O (4 mL), aqueous 40% NaOH (4 mL) and H2O (4 mL)
- filtrationThe resultant slurry is then filtered through celite and MgSO4
- concentrationThe filtrate is then concentrated
- custompurified by silica gel flash column chromatography