反应详情

A mixture of glyoxylic acid monohydrate (4.6 g, 50 mmol) and 4-chloroacetophenone (15.4 g, 0.1 mol) are heated at +95° C. under reduced pressure (50 mbar) for 3 hours. During this time, water is continually removed. After cooling, the reaction mixture is taken up in aqueous sodium carbonate solution and extracted with diethyl ether. The aqueous layer is acidified with 15% hydrochloric acid and extracted with ethyl acetate. The organic layer is dried over sodium sulfate and evaporated, the residue is crystallized from ethyl acetate/hexane to obtain 4-(4-chloro-phenyl)-2-hydroxy-4-oxo-butyric acid.

1. temperatureare heated at +95° C. under reduced pressure (50 mbar) for 3 hours
2. customDuring this time, water is continually removed
3. temperatureAfter cooling
4. extractionextracted with diethyl ether
5. extractionextracted with ethyl acetate
6. dry with materialThe organic layer is dried over sodium sulfate
7. customevaporated
8. customthe residue is crystallized from ethyl acetate/hexane