反应详情

温度

100 °C

A flask was charged with 2-chloro-N-cyclopropylfuro[3,2-d]pyrimidin-4-amine (0.38 g, 1.8 mmol, Example #3, Step C), 7-amino-3-methyl-3,4-dihydroquinolin-2(1H)-one (0.30 g, 1.7 mmol), K2CO3 (0.38 g, 2.7 mmol), Pd2dba3 (0.17 g, 0.18 mmol) and X-Phos (0.17 g, 0.36 mmol) in 1,4-dioxane (20 mL). The flask was evacuated and purged with N2 (3×), and the mixture was heated to about 100° C. overnight. The mixture was cooled to rt and concentrated under reduced pressure to a residue. The residue was purified by preparative TLC (1.0 mm plate), eluting with DCM/MeOH (12:1). The product obtained was further purified by preparative HPLC (Table 2, Method r) to give 7-(4-(cyclopropylamino)furo[3,2-d]pyrimidin-2-ylamino)-3-methyl-3,4-dihydroquinolin-2(1H)-one (0.15 g, 24%): LC/MS (Table 2, Method g) Rt=1.04 min; MS m/z: 177 (M+H)+. Syk IC50=A

1. customThe flask was evacuated
2. custompurged with N2 (3×)
3. temperatureThe mixture was cooled to rt
4. concentrationconcentrated under reduced pressure to a residue
5. customThe residue was purified by preparative TLC (1.0 mm plate)
6. washeluting with DCM/MeOH (12:1)
7. customThe product obtained
8. customwas further purified by preparative HPLC (Table 2, Method r)