反应详情

温度

150 °C

In a microwave reaction vial (S)-2-(2,6-dimethylphenyl)-4-(4-methoxy-3,3-dimethylpiperidin-1-yl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (115 mg, 0.302 mmol), prepared by a method similar to that described by Examples 21-c and 21-d, was combined with methyl isobutyryl acetate (65 mg, 0.45 mmol), toluene (2 mL) and DMAP (7 mg, 0.060 mmol). The vial was heated in a microwave reactor at 150° C. for 30 min. The reaction mixture was then diluted with DCM and water. The layers were separated and the aqueous phase was extracted twice with DCM. The combined organic layers were washed with brine, dried over Na2SO4, filtered, and concentrated. The resulting residue was purified by silica gel flash column chromatography (0-100% 10:1 EtOAc:MeOH/heptanes) to provide (S)-1-(2-(2,6-dimethylphenyl)-4-(4-methoxy-3,3-dimethylpiperidin-1-yl)-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-4-methylpentane-1,3-dione. MS (ESI+) m/z 493.0 (M+H)+

1. customprepared by a method similar to
2. customThe layers were separated
3. extractionthe aqueous phase was extracted twice with DCM
4. washThe combined organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe resulting residue was purified by silica gel flash column chromatography (0-100% 10:1 EtOAc:MeOH/heptanes)