反应详情

To a stirred solution of 4-cyclohexylbenzyl alcohol (1 g, 5.26 mmol) in 45 ml of dry dichloromethane, 5 ml of triethylamine and 41 mg of dimethylaminopyridine was added 1.05 ml (1.25 g) of diphenylphosphinic chloride. The mixture was stirred at room temperature for 3 h after which it was concentrated to approximately 10 ml. The mixture was diluted with dichloromethane, washed with cold 10% sodium bicarbonate, water, dried (sodium sulfate), filtered and concentrated to approximately 10 ml. The resulting solution was chromatographed on silica gel, eluting with ethyl acetate/heptane to provide 1.92 g of the title compound.

1. concentrationwas concentrated to approximately 10 ml
2. additionThe mixture was diluted with dichloromethane
3. washwashed with cold 10% sodium bicarbonate, water
4. dry with materialdried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated to approximately 10 ml
7. customThe resulting solution was chromatographed on silica gel
8. washeluting with ethyl acetate/heptane