HRID1468755
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
2-(tert-Butyldimethylsilanyloxy)-1-phenylethanone (8.0 g, 32 mmol), ethylene glycol (1.99 g, 32 mmol), and p-toluenesulfonic acid (50 mg) was suspended in benzene (50 ml). The mixture was stirred under reflux for 5 hours. The solvent was evaporated under reduced pressure. The residue was treated with water and ethyl acetate. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The crude was purified by silica gel column chromatography (eluent; hexane/ethyl acetate=1/1) to give tert-butyldimethyl-(2-phenyl-[1,3]dioxolan-2-yl-methoxy)silane (5.5 g, 18.7 mmol, 58%) as a yellow oil.
WORKUP
后处理
- temperatureunder reflux for 5 hours
- customThe solvent was evaporated under reduced pressure
- additionThe residue was treated with water and ethyl acetate
- dry with materialThe organic layer was dried over sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe crude was purified by silica gel column chromatography (eluent; hexane/ethyl acetate=1/1)