反应详情

A mixture of 2-methylcyclohexanone (13.1 g), (2R,4R)-2,4-pentanediol (12.2 g), pyridinium p-toluene sulfonate (119 mg) and toluene (120 ml) was refluxed with heating for 8 hours. The reaction mixture was added with a saturated aqueous solution of sodium hydrogen carbonate, extracted with diethyl ether, the organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent: hexane/ethyl acetate=100/0 to 0/100 gradient) to obtain 18.0 g of (2R,4R)-2,4,7-trimethyl-1,5-dioxaspiro[5.5]undecane

1. temperaturewas refluxed
2. temperaturewith heating for 8 hours
3. extractionextracted with diethyl ether
4. dry with materialthe organic layer was dried over sodium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was purified by silica gel chromatography (elution solvent: hexane/ethyl acetate=100/0 to 0/100 gradient)