反应详情

5.37 g (18.86 mmol) of 4-(3-chloro-2-methoxy-4-methylphenyl)-4-methyl-2-oxo-pentanoic acid is dissolved in 112 ml of ethanol, mixed with 2 ml of concentrated sulfuric acid and refluxed for five hours. The ethanol is drawn off in a rotary evaporator, and the residue is carefully mixed with saturated sodium bicarbonate solution after 50 ml of water is added. It is extracted twice with ethyl acetate. The combined organic extracts are washed with water and with brine. After drying, and after the dessicant is filtered off and the solvent is spun in, the residue is chromatographed on silica gel (mobile solvent:ethyl acetate/hexane). 4.81 g (81.6%) of the desired compound is isolated.

1. temperaturerefluxed for five hours
2. customThe ethanol is drawn off in a rotary evaporator
3. additionthe residue is carefully mixed with saturated sodium bicarbonate solution after 50 ml of water
4. additionis added
5. extractionIt is extracted twice with ethyl acetate
6. washThe combined organic extracts are washed with water and with brine
7. customAfter drying
8. filtrationafter the dessicant is filtered off
9. customis chromatographed on silica gel (mobile solvent:ethyl acetate/hexane)