HRID963544

反应详情

EQUATION

反应方程式

HRID 963544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

34.9 g of 2-(4,4-difluorobut-3-en-1-yl)malonic acid diethyl ester are added to 50 ml of methanol. 50 g of potassium carbonate dissolved in 150 ml of water are slowly added dropwise at room temperature and then the mixture is heated to reflux temperature and stirred at that temperature for 15 hours. The reaction mixture is concentrated to dryness by evaporation in a rotary evaporator and the residue is treated with concentrated hydrochloric acid until a pH value of 1 has been obtained and then extracted three times using 150 ml of diethyl ether each time. The combined ether phases are dried over sodium sulfate and concentrated by evaporation. The title compound is obtained in the form of a colourless oil.

WORKUP

后处理

  1. additionare slowly added dropwise at room temperature
  2. temperaturethe mixture is heated
  3. temperatureto reflux temperature
  4. concentrationThe reaction mixture is concentrated to dryness by evaporation in a rotary evaporator
  5. additionthe residue is treated with concentrated hydrochloric acid until a pH value of 1
  6. customhas been obtained
  7. extractionextracted three times
  8. dry with materialThe combined ether phases are dried over sodium sulfate
  9. concentrationconcentrated by evaporation