反应详情

Platinum(IV) oxide (30 mg) was added to a solution of 9-[4-(4-fluoro-3-methoxyphenoxy)phenyl]-7-methyl-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide (400 mg) in THF (dry) (15 ml) and MeOH (15 mL). The mixture was stirred at room temperature under hydrogen for 3 hr. Activated carbon was added and the insoluble solid was removed by filtration through silica gel/Celite pad (eluted with EtOAc). Platinum(IV) oxide (30 mg) was added and the mixture was stirred at room temperature under hydrogen overnight. AcOH (10 mL) and platinum(IV) oxide (30 mg) were added and the mixture was stirred at room temperature under hydrogen for 1 day and at 50° C. for 1 day. Activated carbon was added and the insoluble solid was removed by filtration through silica gel/Celite pad (eluted with EtOAc) and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (NH silica gel, eluted with MeOH in EtOAc) and concentrated in vacuo. The residue was crystallized from THF/IPE to give the title compound (30.3 mg) as colorless crystals.

1. additionActivated carbon was added
2. customthe insoluble solid was removed by filtration through silica gel/Celite pad (eluted with EtOAc)
3. additionPlatinum(IV) oxide (30 mg) was added
4. stirringthe mixture was stirred at room temperature under hydrogen overnight
5. additionAcOH (10 mL) and platinum(IV) oxide (30 mg) were added
6. stirringthe mixture was stirred at room temperature under hydrogen for 1 day and at 50° C. for 1 day
7. additionActivated carbon was added
8. customthe insoluble solid was removed by filtration through silica gel/Celite pad (eluted with EtOAc)
9. concentrationthe filtrate was concentrated in vacuo
10. customThe residue was purified by column chromatography (NH silica gel, eluted with MeOH in EtOAc)
11. concentrationconcentrated in vacuo
12. customThe residue was crystallized from THF/IPE