反应详情

温度

-20 °C

To a stirred solution of (3-benzyloxy-4-nitrophenyl)-methanol (11.0 g, 0.042 mol) in anhydrous THF is added triethylamine (8.7 g, 0.86 mol). The mixture is cooled to −20° C., followed by the addition of methanesulfonyl chloride (5.8 g, 0.051 mol) and then stirred at −20° C. for 45 min. To this mixture is added lithium bromide (37.3 g, 0.43 mol) in anhydrous THF (40 mL) over 40 min. followed by stirring at ambient temperature for 2 h. The suspension is concentrated under reduced pressure and diluted with EtOAc and water. The organic phase is washed with brine, dried over MgSO4, filtered and concentrated to afford 2-benzyloxy-4-bromomethyl-1-nitrobenzene as a yellow solid.

1. stirringby stirring at ambient temperature for 2 h
2. concentrationThe suspension is concentrated under reduced pressure
3. additiondiluted with EtOAc and water
4. washThe organic phase is washed with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated