反应详情

A mixture of 2-[5-amino-1-(2-methyl-1H-benzimidazol-5-yl)-1H-pyrazole-4-carbonyl]-1-(benzenesulfonyl)-5-iodo-1H-indole (117 mg), copper (I) cyanide (84 mg), and 1-methyl-2-pyrrolidinone was reacted in a microwave reactor (190° C., 20 minutes). The reaction mixture was poured into a mixed solution of 2 M ammonia water (40 ml), ethyl acetate (60 ml), and methanol (7 ml), and sonicated for five minutes. After ethyl acetate extraction, the extract was washed with water and then dried over anhydrous sodium sulfate. The desiccant was removed by filtration. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (methanol/dichloromethane=0/100 to 20/100) to give 2-[5-amino-1-(2-methyl-1H-benzimidazol-5-yl)-1H-pyrazole-4-carbonyl]-1-(benzenesulfonyl)-1H-indole-5-carbonitrile (87 mg, 89%).

1. customwas reacted in a microwave reactor (190° C., 20 minutes)
2. customsonicated for five minutes
3. extractionAfter ethyl acetate extraction
4. washthe extract was washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. customThe desiccant was removed by filtration
7. concentrationThe filtrate was concentrated under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography (methanol/dichloromethane=0/100 to 20/100)