反应详情

To a solution of N-(5-methyl-1H-pyrazol-3-yl)-2-(methylthio)-6-morpholin-4-yl-5-nitropyrimidin-4-amine (Intermediate 57, 118 mg) in MeOH (2 ml) and DCM (2 ml) were added Oxone® (302 mg) and NaHCO3 (56 mg) and the resulting mixture was stirred at ambient temperature for 16 hours. [(1S)-1-(5-fluoropyridin-2-yl)ethyl]amine (Intermediate 8, 250 mg) and DIPEA (3 ml) were added and the resulting mixture was stirred at ambient temperature for 3 hours. The mixture was diluted with H2O and EtOAc and the aqueous layer was extracted with EtOAc (4×). The combined organic layers were washed with brine, saturated NaHCO3 (aq) solution, dried and evaporation of the volatiles under reduced pressure gave a colored residue. Purification by column chromatography (60% EtOAc/hexanes) gave the title compound (220 mg). LCMS: 444 [M+1].

1. stirringthe resulting mixture was stirred at ambient temperature for 3 hours
2. extractionthe aqueous layer was extracted with EtOAc (4×)
3. washThe combined organic layers were washed with brine, saturated NaHCO3 (aq) solution
4. customdried
5. customevaporation of the volatiles under reduced pressure
6. customgave a colored residue
7. customPurification by column chromatography (60% EtOAc/hexanes)