Reaktion #481
ord-d106e5c0510845f092f0e721b9abc1a2
Reaktionsgleichung
Lösungsmittel
Reaktionsbedingungen
Vorschrift
Charged a round-bottom flask with a mixture of 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (0.76 g, 3.72 mmol), (R)-8-chloro-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (1.022 g, 3.72 mmol), palladium (II) acetate (0.025 g, 0.11 mmol), rac-BINAP (0.116 g, 0.19 mmol), potassium carbonate (0.926 g, 6.70 mmol), and toluene (15 mL). The atmosphere was inerted through consecutive vacuum-nitrogen purge cycles, then heated at 110 °C under N2(g) for 16 hours. HPLC-UV shows a small percentage (3-6% depending on wavelength) of oxazepine remaining, aminopyridine if fully converted. The mixture was allowed to cool to room temperature. DCM and 2M HCl was added and the orgaic phase were removed. The aqueous phase were basified using solid KOH and a 4M solution. Extracted with DCM, dried oved MgSO4 and concentrated.