반응 #479
ord-b30e73dcf3ae428d887dca581acb0b4f
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Charged a round-bottom flask with a mixture of 6-methoxy-5-(1-methyl-1H-pyrazol-4-yl)pyridin-2-amine (4.5 g, 22.03 mmol), (R)-8-chloro-4-methyl-2-phenyl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (6.05 g, 22.03 mmol), palladium (II) acetate (0.148 g, 0.66 mmol), rac-BINAP (0.686 g, 1.10 mmol), potassium carbonate (4.57 g, 33.05 mmol), and toluene (90 mL). The atmosphere s inerted through itrogen purge cycles, then heated at 120 °C or 16 hours. HPLC-UV shows <5% of starting materials remaining. The heating block was removed and the mixture was allowed to cool to room temperature. Added 300 mL dichloromethane and adjusted the pH to 2 with 2.0N aqueous HCl. Separated the phases and basified the aqueous with 1.0N aqueous sodium hydroxide. Extracted with 200 mL DCM, followed by a second extraction with 100 mL DCM. The organics were dried with magnesium sulfate and concentrated by rotary evaporator to give EN04092-39-001 (9.90g, 22.37 mmol, 102%) name='[Samples]' index='0' field='Samples' type='field' length='9'/>ber- coloured foam.