反应详情

温度

140 °C

A microwave vessel was charged with (2-bromo-3-methylphenyl)(pyrrolidin-1-yl)methanone (0.081 g, 0.301 mmol), dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (0.018 g, 0.038 mmol), Pd2(dba)3 (0.018 g, 0.020 mmol), potassium phosphate (0.106 g, 0.502 mmol), 2-amino-7-fluoro-3-morpholinoquinolin-6-ylboronic acid (0.073 g, 0.251 mmol), dioxane (1.6 mL) and water (0.8 mL). The vessel was purged with argon, sealed and heated by microwave radiation at 140° C. for 15 min. The mixture was concentrated, diluted with EtOAc (10 mL) and the suspension was filtered through celite rinsing with EtOAc. The filtrate was washed with saturated brine (5 mL), dried over sodium sulfate and concentrated. The material was purified by column chromatography on silica gel (33 mL) which had been deactivated with Et3N (3.3 mL) eluting with 1.5% MeOH/EtOAc to afford (2-(2-amino-7-fluoro-3-morpholinoquinolin-6-yl)-3-methylphenyl)(pyrrolidin-1-yl)methanone. MS (ESI, pos. ion) m/z: 435 (M+1).

1. customThe vessel was purged with argon
2. customsealed
3. concentrationThe mixture was concentrated
4. additiondiluted with EtOAc (10 mL)
5. filtrationthe suspension was filtered
6. washthrough celite rinsing with EtOAc
7. washThe filtrate was washed with saturated brine (5 mL)
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated
10. customThe material was purified by column chromatography on silica gel (33 mL) which
11. washeluting with 1.5% MeOH/EtOAc