HRID1969379
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
To a mixture of (S)-5-(hydroxymethyl)-dihydrofuran-2(3H)-one (1.78 g, 0.0153 mol) and 3,4-dihydro-2H-pyran (2.62 g, 0.0312 mol, Alfa) in 40 mL of CH2Cl2 was added PPTS (0.391 g, 0.00156 mol, Aldrich) slowly. After stirring at rt overnight, the reaction mixture was quenched with 5 mL of water. The mixture was extracted with EtOAc (50 mL×2). The combined organic phases were dried over Na2SO4 and concentrated in vacuo to give pale yellow oil. The crude product was purified by a silica gel column chromatography (3:1 (v/v) petroleum ether/EtOAc) to afford the title compound as colorless oil (2.7 g, 88%).
WORKUP
后处理
- customthe reaction mixture was quenched with 5 mL of water
- extractionThe mixture was extracted with EtOAc (50 mL×2)
- dry with materialThe combined organic phases were dried over Na2SO4
- concentrationconcentrated in vacuo
- customto give pale yellow oil
- customThe crude product was purified by a silica gel column chromatography (3:1 (v/v) petroleum ether/EtOAc)