反应详情

A mixture of (R)-1-(4-(6-benzyl-2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-yl)-3-methylpiperazin-1-yl)ethanone (0.35 g, 0.539 mmol), acetic acid (0.154 mL, 2.70 mmol), THF (9 mL) and H2O (3 mL) was degassed via vacuum and recharged with nitrogen gas (2×). Then 20 mol % Pd(OH)2/carbon (0.114 g, 0.162 mmol) was added and the mixture was degassed via vacuum and placed under an atmosphere of hydrogen. The mixture was stirred at rt under H2 atmosphere via balloon for 2 h and then filtered. The solution was then diluted with EtOAc and washed with sat aq NaHCO3. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated to provide (R)-1-(3-methyl-4-(2-(3-methyl-1-tosyl-1H-indol-4-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-yl)piperazin-1-yl)ethanone, which was used without the need for further purification. MS (ESI+) m/z 559.3 (M+H)+.

1. customwas degassed via vacuum
2. customthe mixture was degassed via vacuum
3. filtrationfiltered
4. additionThe solution was then diluted with EtOAc
5. washwashed with sat aq NaHCO3
6. washThe organic layer was washed with brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated