反应详情

温度

0 °C

{4-[3-(benzyloxy)propyl]benzyl alcohol (1.86 g, 7.31 mmol) was dissolved in 82 mL dichloromethane. The solution was cooled to 0° C. 3.25 g (12.41 mmol) triphenyl phosphine and 4.11 g (12.41 mmol) carbon tetrabromide were added to the solution. The ice bath was removed and the reaction was stirred for 1 h. The solution was concentrated in vacuo, to the residue was added tert-butyl methyl ether (100 mL) and the mixture was stirred at −20° C. for 30 min. The mixture was filtrated and the filtrate was concentrated in vacuo. The crude product was purified on silica gel using a hexane/ethyl acetate gradient, and the appropriate fractions were combined and concentrated.

1. customThe ice bath was removed
2. concentrationThe solution was concentrated in vacuo, to the residue
3. additionwas added tert-butyl methyl ether (100 mL)
4. stirringthe mixture was stirred at −20° C. for 30 min
5. filtrationThe mixture was filtrated
6. concentrationthe filtrate was concentrated in vacuo
7. customThe crude product was purified on silica gel using a hexane/ethyl acetate gradient
8. concentrationconcentrated