HRID341649

反应详情

EQUATION

反应方程式

HRID 341649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of mercury (II) acetate (7.76 g, 0.024 mol), sulfuric acid (9 ml, 0.09 mol) and water (450 ml) is heated at 60° C. 2-(1,1-dimethylprop-2-ynyloxy)propionic acid methyl ester (90 g, 0.529 mol) is added carefully at 60° C. The reaction mixture is maintained at 60° C. for 8 hours and cooled to ambient temperature. The aqueous phase is extracted with diethyl ether (3×250 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-(1,1-dimethyl-2-oxopropoxy)propionic acid methyl ester (24 g) as a colorless oil.

WORKUP

后处理

  1. temperatureThe reaction mixture is maintained at 60° C. for 8 hours
  2. temperaturecooled to ambient temperature
  3. extractionThe aqueous phase is extracted with diethyl ether (3×250 ml)
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationThe mixture is filtered
  7. customthe filtrate is evaporated under reduced pressure
  8. customThe residue is purified by column chromatography on silica gel