反应详情

3-Benzyloxymethyl-1-{4-[4-(5-cyclopropyl-3-methylpyridin-2-yl)piperazine-1-carbonyl]-3-fluorophenyl}-5-methylimidazolidine-2,4-dione (270 mg) described in Example 536 was dissolved in methanol (20 mL), formic acid (0.36 ml) and 10% palladium carbon catalyst (108 mg) were added, and the mixture was stirred with heating under reflux for 16 hr. The reaction mixture was cooled, the catalyst was removed by celite filtration, and the solvent was evaporated. To the residue were added methanol and 0.5N aqueous sodium hydroxide solution, and the mixture was stirred at room temperature. The reaction solution was neutralized with acetic acid, and the solvent was evaporated. Water was added to the residue, and the mixture was extracted with chloroform. The organic layer was dried over sodium sulfate, and the solvent was evaporated. The obtained residue was purified by column chromatography (chloroform:methanol) to give the title compound (40 mg).

1. temperaturewith heating
2. temperatureunder reflux for 16 hr
3. temperatureThe reaction mixture was cooled
4. customthe catalyst was removed by celite filtration
5. customthe solvent was evaporated
6. additionTo the residue were added methanol and 0.5N aqueous sodium hydroxide solution
7. stirringthe mixture was stirred at room temperature
8. customthe solvent was evaporated
9. additionWater was added to the residue
10. extractionthe mixture was extracted with chloroform
11. dry with materialThe organic layer was dried over sodium sulfate
12. customthe solvent was evaporated
13. customThe obtained residue was purified by column chromatography (chloroform:methanol)