反应详情

温度

90 °C

To a solution of 4-(3-bromo-5-chlorophenoxy)-5-chloro-1H-benzimidazole 430 mg, 1.201 mmol) in DMF (5 mL) was added palladium tetrakistriphenylphosphine (416 mg, 0.360 mmol) and zinc cyanide (141 mg, 1.201 mmol) and the mixture heated to 90° C. for 1 hour. This mixture was partitioned between ethyl acetate (50 mL) and water (20 mL). The organic extract was washed with water (10 mL), dried over MgSO4, filtered and the solvent removed in vacuo. This residue was purified on silica gel eluting with 0-20% ethyl acetate/methylene chloride to give the title compound. LRMS (M+1)=303.8.

1. customThis mixture was partitioned between ethyl acetate (50 mL) and water (20 mL)
2. extractionThe organic extract
3. washwas washed with water (10 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customThis residue was purified on silica gel eluting with 0-20% ethyl acetate/methylene chloride