反应详情

In a reaction vial, 5-bromo-1H-pyrrolo[2,3-b]pyridine (55, 287 mg, 1.46 mmol), 2-methyl-propane-1-sulfonic acid (2,4-difluoro-3-formyl-phenyl)-amide (59, 445 mg, 1.60 mmol) and potassium hydroxide (246 mg, 4.38 mmol) are combined with 7 mL of methanol and stirred at room temperature overnight. The reaction was combined with ethyl acetate and aqueous saturated sodium chloride, and extracted. The organic layer was washed with water, brine, and dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum. The residue was treated with 75 mL of acetonitrile:water 4:1 with 5% trifluoroacetic acid and stirred overnight at room temperature. The reaction was combined with ethyl acetate and aqueous saturated sodium chloride, and extracted. The organic layer was washed with water, brine, and dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum to provide the desired compound (68, 618 mg).

1. extractionextracted
2. washThe organic layer was washed with water, brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under vacuum
6. additionThe residue was treated with 75 mL of acetonitrile:water 4:1 with 5% trifluoroacetic acid
7. stirringstirred overnight at room temperature
8. extractionextracted
9. washThe organic layer was washed with water, brine
10. dry with materialdried over magnesium sulfate
11. filtrationfiltered
12. concentrationthe filtrate concentrated under vacuum