反应详情

温度

50 °C

To a solution of 5-{2-[(6-chloroquinolin-4-yl)methyl]-7-cyclopropylmethyl-4,6-dioxo-4,5,6,7-tetrahydro-2H-pyrazolo[3,4-d]pyrimidin-3-yl}-1-methyl-1H-pyrrole-3-carbonitrile (0.42 g) in pyridine (5 mL) were added 4-chlorophenyl phosphorodichloridate (0.5 mL) and 3-nitro-1,2,4 triazole (0.15 g). After heating (Tb=50° C.) for 3 h, the reaction was diluted with ethyl acetate. The organic solution was washed with saturated NaHCO3 and brine, dried (Na2SO4), filtered and concentrated. The residue was dissolved in THF (10 mL) and ethanolamine (1.0 mL). After 3 h, the reaction was concentrated. This residue was purified by flash chromatography using a FlashMaster™ yielding 0.22 g, ES (M+H)+=529.

1. washThe organic solution was washed with saturated NaHCO3 and brine
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in THF (10 mL)
6. concentrationthe reaction was concentrated
7. customThis residue was purified by flash chromatography
8. customyielding 0.22 g, ES (M+H)+=529