HRID1729245
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
PROCEDURE
实验过程
0.8 g of sodium hydride (60% dispersion in mineral oil) was added over 5 minutes under ice-cooling to a solution of 3.64 g of 9-fluorenol and 3 ml of ethyl bromoacetate in 40 ml of N,N-dimethylformamide. After stirring for 50 minutes, the reaction mixture was poured into ice-cold 5% HCl and extracted with ether. The organic layer was washed with a saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by a silica gel column chromatography (eluting solution: methylene chloride-hexane) to give 2.28 g of ethyl 9-fluorenyloxyacetate.
WORKUP
后处理
- extractionextracted with ether
- washThe organic layer was washed with a saturated saline
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe residue was purified by a silica gel column chromatography (eluting solution: methylene chloride-hexane)