HRID1827520
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 solution of 3-hydroxy-benzaldehyde (6.51 g, 53.3 mmol) and 3,4-dihydro-2H-pyran (7.3 mL, 80.0 mmol) in 150 mL methylene chloride was added pyridinium p-toluenesulfonate (1.34 g, 5.33 mmol). The reaction mixture was stirred at room temperature overnight. The layers were separated and the organic layer was washed with saturated aqueous sodium bicarbonate. The organic layer was dried (magnesium sulfate), filtered, and concentrated. Medium pressure silica gel chromatography of the residue (5% ethyl acetate/hexanes to 10% ethyl acetate/hexanes) aforded 10.34 g (94%) of the title compound of Step A.
WORKUP
后处理
- customThe layers were separated
- washthe organic layer was washed with saturated aqueous sodium bicarbonate
- dry with materialThe organic layer was dried (magnesium sulfate)
- filtrationfiltered
- concentrationconcentrated