反应详情

A solution of 4-(3-bromophenyl)butan-1-ol (5 g) (WO 0266422 A1) in dry DMF was treated with imidazole (1.8 g) and tert-butyldiphenylsilyl chloride (7.2 g) and stirred at room temperature for 16 h. The reaction mixture was partitioned between water and EtOAc. The organic phase was washed with 2M HCl, water, sat. NH4Cl(aq), water, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography (SPE, Gradient between cyclohexane and cyclohexane-EtOAc (5:1) to give the title compound. LCMS RT=4.82 min

1. customThe reaction mixture was partitioned between water and EtOAc
2. washThe organic phase was washed with 2M HCl, water, sat. NH4Cl(aq), water
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe residue was purified by chromatography (SPE, Gradient between cyclohexane and cyclohexane-EtOAc (5:1)