反应详情

To a mixture of 5-{[(2R)-1-benzylpyrrolidin-2-yl]methoxy}-6-ethyl-3-({4-[4-(4-methylpiperazin-1-yl)piperidin-1-yl]phenyl}amino)pyrazine-2-carboxamide (182 mg), and acetic acid (3 mL) was added 10% palladium-supported carbon (53% wet product) (63 mg), followed by stirring for 6 hours under a hydrogen gas atmosphere (4 atm). The reactant was filtered through celite, then the mixture was concentrated under reduced pressure, and a saturated aqueous sodium hydrogen carbonate solution was added thereto, followed by extraction with a mixed solvent of chloroform:methanol=8:2. The organic phase was washed with saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH2 type: eluent; chloroform:methanol=98:2) to obtain 6-ethyl-3-({4-[4-(4-methylpiperazin-1-yl)piperidin-1-yl]phenyl}amino)-5-[(2R)-pyrrolidin-2-ylmethoxy]pyrazine-2-carboxamide (138 mg) as a yellow solid.

1. filtrationThe reactant was filtered through celite
2. concentrationthe mixture was concentrated under reduced pressure
3. additiona saturated aqueous sodium hydrogen carbonate solution was added
4. extractionfollowed by extraction with a mixed solvent of chloroform
5. washThe organic phase was washed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe obtained residue was purified by silica gel column chromatography (NH2 type: eluent; chloroform:methanol=98:2)