反应详情

温度

90 °C

A 500 ml tube was charged with 6-bromo-7-methoxy-1H-benzoimidazole (36 g, 0.16 mol, 1.0 equiv.), dihydropyran (40.01 g, 0.48 mol, 3.0 equiv.) and pyridinium-p-toluenesulfonate (7.96 g, 0.032 mol, 0.2 equiv.) in EtOAc (400 mL), sealed and the reaction mixture was heated at 90° C. overnight. The reaction mixture was concentrated in vacuo and the crude product was purified by SiO2 chromatography eluting with an EtOAc/hexane gradient (30-40% EtOAc) to afford 5-bromo-4-methoxy-1-(tetrahydro-pyran-2-yl)-1H-benzoimidazole (30 g, 60% yield) as a brown solid.

1. customsealed
2. concentrationThe reaction mixture was concentrated in vacuo
3. customthe crude product was purified by SiO2 chromatography
4. washeluting with an EtOAc/hexane gradient (30-40% EtOAc)