反应详情

Compound 18-1 (2.00 g) was dissolved in methylene chloride (50 ml), triphenylphosphine (2.97 g) and N-bromosuccinimide (1.99 g) were added under ice-cooling, and the mixture was stirred under ice-cooling for 1 hr, and further at room temperature for 15 hr. The reaction mixture was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Diethyl ether (100 ml) was added, and the precipitated triphenylphosphine oxide was filtered off. The concentrate of the filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=5:1-3:1) to give the object product (2.17 g) as a pale-brown oil.

1. temperaturecooling
2. temperaturecooling for 1 hr
3. washThe reaction mixture was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. additionDiethyl ether (100 ml) was added
7. filtrationthe precipitated triphenylphosphine oxide was filtered off
8. concentrationThe concentrate of the filtrate
9. customwas purified by silica gel column chromatography (hexane:ethyl acetate=5:1-3:1)