HRID4172

反应详情

EQUATION

反应方程式

HRID 4172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

187 g (0.88 mol) of diethyl 2-methyl-2-propargyl-malonate are added to a solution of 101 g (1.8 mol) of potassium hydroxide in a mixture of 560 ml of water/ethanol (1:1) and the mixture is refluxed with stirring for 2 hours. After the reaction has ended (monitored by TLC) the mixture is evaporated to dryness in vacuo and the residue is then taken up with in water. The aqueous solution is acidified with 50% sulphuric acid and extracted several times with methylene chloride. The combined extracts are dried, evaporated to dryness in vacuo and a colourless product is obtained, m.p. 135° C.

WORKUP

后处理

  1. temperaturethe mixture is refluxed
  2. customis evaporated to dryness in vacuo
  3. extractionextracted several times with methylene chloride
  4. customThe combined extracts are dried
  5. customevaporated to dryness in vacuo
  6. customa colourless product is obtained