Acetonitrile → HCID 11305148, compound

Participants

Reaction Conditions

Reaction Steps

To 10 mL of degazed acetonitrile, 5-(3-bromo-phenyl)-8-methoxy-1-methyl-7-phenyl-1,3-dihydro-benzo[e][1,4]diazepin-2-one Example 62 (200 mg, 0.46 mmol), phenylacetylene (715 μL, 2.30 mmol), copper iodide (15 mg, 0.08 mmol), triphenylphosphine (30 mg, 0.11 mmol), PdCl2 (10 mg, 0.06 mmol) and triethylamine (0.9 mL) were added. The mixture was stirred for 16 hours at 50° C. under nitrogen atmosphere. The working solution was evaporated under vacuum. The residue was partitioned from water and ethyl acetate and extracted two more times with ethyl acetate. The organic phase was dried over Na2SO4 and concentrated until dryness. The residue was purified by chromatography (eluant: Hexane/EtOAc: 1/1). The title compound was crystallised from ether/pentane to afford 134 mg of the title compound: beige solid, yield=90%.

Provenance & Evidence