反应详情

To a solution of 1-benzyl-6-chloro-5-iodo-2-methanesulfonyl-1H-benzoimidazole (2.7 g, 6.0 mmol) in DMF (30 ml) was added (5-hydroxy-2-methyl-phenyl)-phosphonic acid diethyl ester (1.9 g, 8.4 mmol), followed by potassium carbonate (1.7 g, 12 mmol). After stirring overnight at rt the volatiles were removed by rotary evaporation. The residue thus obtained was partitioned between EtOAc and half-saturated ammonium chloride solution. The EtOAc layer was washed with H2O, brine, and then dried with MgSO4. The crude oil was then purified by flash chromatrography (SiO2, 80 g) using a gradient up to 65% EtOAc in hexane to yield the title compound.

1. customwere removed by rotary evaporation
2. customThe residue thus obtained
3. customwas partitioned between EtOAc and half-saturated ammonium chloride solution
4. washThe EtOAc layer was washed with H2O, brine
5. dry with materialdried with MgSO4
6. customThe crude oil was then purified by flash chromatrography (SiO2, 80 g)