反应详情

温度

70 °C

To a stirred solution of 9-(benzyloxy)-6-((1-(4-chlorophenyl)cyclopentyl)methyl)-2-(1,1,1-trifluoropropan-2-yl)-3,4-dihydro-1H-pyrazino[1,2-c]pyrimidine-1,8(2H)-dione (44) (90.8 mg, 162 μmol, Eq: 1.00) in methanol (5 ml) was added HCl (conc) (240 mg, 0.2 ml, 6.58 mmol, Eq: 40.6) and the reaction mixture was heated at 70° C. for 18 hrs. The reaction mixture was neutralized with saturated aqueous NaHCO3 solution, extracted with dichloromethane, dried (MgSO4), concentrated, triturated with diethyl ether, filtered, and dried to obtain 6-((1-(4-chlorophenyl)cyclopentyl)methyl)-9-hydroxy-2-(1,1,1-trifluoropropan-2-yl)-3,4-dihydro-1H-pyrazino[1,2-c]pyrimidine-1,8(2H)-dione (45) (pink powder, 40.1 mg, 85.3 μmol, 52.6% yield).

1. extractionextracted with dichloromethane
2. dry with materialdried (MgSO4)
3. concentrationconcentrated
4. customtriturated with diethyl ether
5. filtrationfiltered
6. customdried