Formic Acid → HCID 21459440, compound

Participants

Reaction Steps

The above 4-(3,5-difluorophenyl)-3-cyclohexenyl-1-cyclohexanone propyleneketal (114 g, 327 mmol) was hydrogenated in a mixed solvent of ethyl acetate with ethanol in the presence of Raney Ni catalyst (44.8 g), followed by filtering off the catalyst, distilling off the solvent under reduced pressure, adding to the residue, formic acid (50.0 g, 1.09 mol) and toluene (300 ml), refluxing the mixture for 4 hours, adding water to the reaction solution, washing the organic layer successively with a saturated aqueous solution of sodium bicarbonate and water, drying over magnesium sulfate, distilling off toluene under reduced pressure, and purifying the residue according to column chromatography treatment using toluene as a developing solvent, on silica gel, to obtain 4-(3,5-difluorophenyl)cyclohexyl-1-cyclohexanone (56.8 g, 194 mmol). Yield: 59.3%.

Provenance & Evidence