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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a mixture of potassium tert-butoxide (28.5 g, 0.254 mol) in tetrahydrofuran (200 ml) cooled to 0° C., is added a solution of 2-(1,1-dimethyl-2-oxopropoxy)propionic acid methyl ester (24 g, 0.127 mol) in tetrahydrofuran (50 ml). The reaction mixture is stirred at 0° C. for 3 hours. The reaction mixture is quenched with ice cold water, and the aqueous phase is extracted with diethyl ether (3×200 ml). The organic phases are combined, washed with water, and dried over anhydrous sodium sulfate. The mixture is filtered, and the filtrate is evaporated under reduced pressure. The residue is purified by column chromatography on silica gel to give 2,2,6-trimethylpyran-3,5-dione (7.5 g) as a white solid.
WORKUP
后处理
- customThe reaction mixture is quenched with ice cold water
- extractionthe aqueous phase is extracted with diethyl ether (3×200 ml)
- washwashed with water
- dry with materialdried over anhydrous sodium sulfate
- filtrationThe mixture is filtered
- customthe filtrate is evaporated under reduced pressure
- customThe residue is purified by column chromatography on silica gel