反应详情

41 mg (0.073 mmol) tert-butyl 5-(3,5-dicyano-2,6-dimethyl-1,4-dihydropyridin-4-yl)-3-{[(3-ethoxy-3-oxopropyl)sulfonyl]amino}-1H-indazole-1-carboxylate (Example 19A) were dissolved in dichloromethane (4 ml) and treated with 0.062 ml (0.8 mmol) trifluoroacetic acid. The mixture was stirred at room temperature for 2 h and then concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution. The organic layer was separated, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by preparative RP-HPLC (acetonitrile/water gradient) to give 33 mg (98% of th.) of the title compound.

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with saturated aqueous sodium bicarbonate solution
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by preparative RP-HPLC (acetonitrile/water gradient)