反应详情

To a solution of 1-biphenyl-4-ylmethyl-6-chloro-5-iodo-2-methanesulfonyl-1H-benzoimidazole (1.2 g, 2.3 mmol) in DMF (10 ml) at rt was added K2CO3 (635 mg, 4.6 mmol), followed by (5-hydroxy-2-methyl-phenyl)-phosphonic acid diethyl ester (630 mg, 2.6 mmol). The mixture was stirred overnight at rt. The solvent was then removed on a rotary evaporator. The resulting residue was partitioned between EtOAc and a solution of half-saturated ammonium chloride. The EtOAc layer was washed with H2O, brine, and then dried with MgSO4. After rotary evaporation, the residue was purified by flash chromatography (SiO2, 12 g). The title compound was eluted with a gradient up to 50% EtOAc in Hexane as a mixture of the two protected regioisomers.

1. customThe solvent was then removed on a rotary evaporator
2. customThe resulting residue was partitioned between EtOAc
3. washThe EtOAc layer was washed with H2O, brine
4. dry with materialdried with MgSO4
5. customAfter rotary evaporation
6. customthe residue was purified by flash chromatography (SiO2, 12 g)
7. washThe title compound was eluted with a gradient up to 50% EtOAc in Hexane as a mixture of the two protected regioisomers