反应详情

9-Benzyloxy-6-(2,6-dichlorobenzyl)-2-isopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (65) (0.04 g, 84.7 μmol, Eq: 1.00) was suspended in methanol (0.5 ml) and HCl conc (600 mg, 0.5 ml, 16.5 mmol, Eq: 194) was added. The resulting mixture was stirred at room temperature overnight. The organic solvent was mostly removed. Aqueous NaHCO3 was added slowly. The water was removed under reduced pressure. The residue was taken up in ethanol and stirred at room temperature overnight. The suspension was filtered and the filtrate was concentrated to dryness. The remaining solid was purified by reverse phase flash chromatography (13 g C18, water/acetonitrile 0-100% acetonitrile). Product containing fractions were combined and lyophilized to of ford 6-(2,6-dichlorobenzyl)-9-hydroxy-2-isopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (66) (0.01 g, 30.6% yield) as a white solid.

1. customThe organic solvent was mostly removed
2. additionAqueous NaHCO3 was added slowly
3. customThe water was removed under reduced pressure
4. stirringstirred at room temperature overnight
5. filtrationThe suspension was filtered
6. concentrationthe filtrate was concentrated to dryness
7. customThe remaining solid was purified by reverse phase flash chromatography (13 g C18, water/acetonitrile 0-100% acetonitrile)
8. additionProduct containing fractions