HRID376294
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
A mixture of 3.10 g of 6-[1,3]dioxolan-2-yl-pyridine-2-carbaldehyde (17.3 mmol), 9.26 g of (methyl)triphenylphosphonium bromide (25.9 mmol) and 4.80 g of potassium carbonate (34.8 mmol) in 60 ml of 1,4-dioxane is maintained under reflux for 5 hours. The solid is removed by filtration and then the solvent is evaporated off. The residue is taken up in ethyl acetate, the solution is washed with water and then with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and filtered. After evaporation of the solvent, the title compound is isolated by chromatography on a silica column (eluent: hexane/ethyl acetate; 80:20). 1.63 g of a yellow oil are obtained.
WORKUP
后处理
- temperatureis maintained
- temperatureunder reflux for 5 hours
- customThe solid is removed by filtration
- customthe solvent is evaporated off
- washthe solution is washed with water
- dry with materialwith a saturated aqueous solution of sodium chloride, dried over magnesium sulfate
- filtrationfiltered
- customAfter evaporation of the solvent