反应详情

温度

130 °C

A mixture of 6-bromo-4-((1S,2S)-2-hydroxy-2-methylcyclohexylamino)pyrrolo[1,2-b]pyridazine-3-carboxamide (31 mg, 0.084 mmol), phenylboronic acid (21 mg, 0.17 mmol), Pd(OAc)2 (1.0 mg, 0.004 mmol), and dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (X-Phos, 4 mg, 0.0084 mmol) in DMF (0.5 mL) were added 2M K3PO4 (0.13 mL, 0.25 mmol) and the solution degassed via N2 sparging. The mixture was sealed and heated at 130° C. for 30 min. The reaction was cooled and the product was isolated via preparative HPLC to afford the title compound (17.5 mg, 52% yield) as a pale yellow solid. LCMS: 365.15 (M+H)+; HPLC (condition L): retention time=8.34 min; 1H NMR (methanol-d4, 400 MHz) δ 8.16 (s, 1H), 7.94 (d, J=1.7 Hz, 1H), 7.70 (m, 2H), 7.41 (t, J=7.5 Hz, 2H), 7.27 (m, 2H), 4.35 (m, 1H), 2.21 (m, 2H), 1.50-1.88 (m, 6H), 1.35 (s, 3H).

1. customthe solution degassed via N2 sparging
2. customThe mixture was sealed
3. temperatureThe reaction was cooled
4. customthe product was isolated via preparative HPLC