反应详情

A solution of (4′-bromo-biphenyl-4-yl)-methanol, 7.01 g (27.9 mmol) and dibromo-triphenylphosphorane 11.8 g (27.9 mmol) in 150 mL of methylene chloride stirred at room temperature for 2 h. The solution was diluted with 100 mL of water and extracted with 2×200 mL portions of diethyl ether. The organic layers were combined, washed with sat. aq. NaCl, and dried (MgSO4). After the solution was concentrated, the residue was purified through a short plug of silica gel (eluted with 50% EtOAc-Heptane) to afford the desired product in 9.1 g (100%) as a white solid. The material was taken to the next step without further purification.

1. extractionextracted with 2×200 mL portions of diethyl ether
2. washwashed with sat. aq. NaCl
3. dry with materialdried (MgSO4)
4. concentrationAfter the solution was concentrated
5. customthe residue was purified through a short plug of silica gel (eluted with 50% EtOAc-Heptane)