反应详情

A solution of 16.1 g of potassium hydroxide in 250 ml of ethanol is added dropwise to 87 g of 4-phenoxybutylmalonic acid diethyl ester in 250 ml of ethanol at room temperature. The mixture is stirred for 24 hours and substantially concentrated in vacuo; the residue is taken up in 500 ml of water and the aqueous mixture is extracted with 200 ml of diethyl ether. The aqueous phase is acidified with concentrated hydrochloric acid, while cooling with ice, and extracted 3 times with 200 ml of diethyl ether each time. After drying over sodium sulfate, the organic phase is concentrated. 66.45 g of 4-phenoxybutylmalonic acid ethyl ester of m.p. 69° to 72° C. are obtained.

1. concentrationsubstantially concentrated in vacuo
2. extractionthe aqueous mixture is extracted with 200 ml of diethyl ether
3. temperaturewhile cooling with ice
4. extractionextracted 3 times with 200 ml of diethyl ether each time
5. dry with materialAfter drying over sodium sulfate
6. concentrationthe organic phase is concentrated