反应详情

温度

80 °C

A mixture of 6-benzyl-2,4-dichloro-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (0.655 g, 1.89 mmol), (R)-1-(3-methylpiperazin-1-yl)ethanone 2,2,2-trifluoroacetate (1 g, 2.84 mmol) and DIEA (2.65 mL, 15.2 mmol) in i-PrOH (25 mL) was heated to 80° C. for 48 h. The reaction mixture was then diluted with EtOAc, and washed successively with sat aq NaHCO3 and brine. The organic layer was then dried over Na2SO4, filtered and concentrated. The resulting residue was diluted with DCM and filtered to remove solid. The filtrate was concentrated and purified by FCC (0-5% MeOH in DCM) to provide (R)-1-(4-(6-benzyl-2-chloro-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-yl)-3-methylpiperazin-1-yl)ethanone. MS (ESI+) m/z 400.3 (M+H)+.

1. washwashed successively with sat aq NaHCO3 and brine
2. dry with materialThe organic layer was then dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. additionThe resulting residue was diluted with DCM
6. filtrationfiltered
7. customto remove solid
8. concentrationThe filtrate was concentrated
9. custompurified by FCC (0-5% MeOH in DCM)