反应详情

A mixture of dimeric 2-hydroxycyclohexanone (13.7 g), 2-benzyloxyethanol (20 g) and p-toluensulphonic acid (2 g) were dissolved in xylene (500 ml) in a round bottom flask fitted with a Dean Stark apparatus and reluxed for 10 hrs. The resulting solution was cooled, washed with sodium hydrogen carbonate (3×50 ml) dried and concentrated under reduced pressure. The crude oil was then pruified by flash chromatography using cyclohexane/ethyl acetate 60/40 as eluant yielding 20 g of the title compound (RF=0.5).

1. customfitted with a Dean Stark apparatus
2. temperatureThe resulting solution was cooled
3. washwashed with sodium hydrogen carbonate (3×50 ml)
4. customdried
5. concentrationconcentrated under reduced pressure