反应详情

50 g of 4-(2-ethoxycarbonyl-4-methyl-3-oxo-pent-1-enyl)benzoic acid are dissolved in 300 ml of THF, 1.00 g of palladium on carbon (10%) is added, and the mixture is hydrogenated under a hydrogen pressure of 4 bar in an autoclave for 24 h. The mixture is diluted with dichloromethane and filtered with suction through Celite, the residue is washed with dichloromethane and concentrated in vacuo. The residue is purified by chromatography on silica gel (ethyl acetate/n-heptane=3/1). 45 g of compound 45 are obtained as an oil. C16H20O5 (292.3) MS (ESI+): 293.1 (M+H)+, tR=1.37 min (Gradient 2).

1. customfor 24 h
2. filtrationfiltered with suction through Celite
3. washthe residue is washed with dichloromethane
4. concentrationconcentrated in vacuo
5. customThe residue is purified by chromatography on silica gel (ethyl acetate/n-heptane=3/1)