Reaktion #475
ord-621d036677ca44618570da1795ad36a5
Reaktionsgleichung
Lösungsmittel
Reaktionsbedingungen
Vorschrift
Charged a standard microwave vial with a mixture of 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (0.500 g, 2.45 mmol), (R)-8-chloro-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.611 g, 2.22 mmol), palladium (II) acetate (0.015 g, 0.07 mmol), rac-BINAP (0.069 g, 0.11 mmol), potassium carbonate (0.461 g, 3.34 mmol), and toluene (20 mL). The atmosphere was inerted through consecutive vacuum-nitrogen purge cycles, then heated at 120 °C for 16 hours. HPLC-UV shows some starting materials remaining (<11% at 254 nm). The mixture was cooled to room temperature and 20 mL of DCM was added to the vessel. The pH was adjusted to pH 2 with 2.0N aqueous HCl and the phases were separated. Basified the aqueous with 2.0 M aqueous NaOH and extracted with 2 X 30 mL DCM. The organics were combined, dried with magnesium sulfate and concentrated by rotary evaporator to yield EN04092-36-001 (811 mg, 1.833 mmol, 82 %).