반응 #4268

반응 방정식

diethyl 2-methyl-2-propargyl-malonate

potassium hydroxide

→

2-Methyl-2-propargyl-malonic acid

용매

water ethanol

반응 조건

후처리

1. 1
   온도the mixture is refluxed
2. 2
   기타is evaporated to dryness in vacuo
3. 3
   추출extracted several times with methylene chloride
4. 4
   기타The combined extracts are dried
5. 5
   기타evaporated to dryness in vacuo
6. 6
   기타a colourless product is obtained

실험 절차

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.

출처