HRID341650

反应详情

EQUATION

反应方程式

HRID 341650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe reaction mixture is quenched with ice cold water
  2. extractionthe aqueous phase is extracted with diethyl ether (3×200 ml)
  3. washwashed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationThe mixture is filtered
  6. customthe filtrate is evaporated under reduced pressure
  7. customThe residue is purified by column chromatography on silica gel