Triethylamine → HCID 22099750, compound

Participants

Reaction Steps

To a solution of 0.20 mol of 1,4,5,6-tetrahydropyrazolo[4,3-d][1]benzazepine, 0.80 mol of triethylamine is added 0.42 mol of 6-[(5-fluoro-2-methylbenzoyl)amino]pyridine-3-carbonyl chloride in 15 ml of dichloromethane. The mixture is stirred under argon for 16 hours and diluted with dichloromethane (25 ml). The mixture is washed with H2 O), 1MNaHCO3, brine and dried (Na2SO4). The solvent is removed and the residue in methanol-tetrahydrofurane(1:1) stirred with 1NNaOH for 5 hours. The mixture is neutralized with acetic acid and the solvent removed. To the residue is added H2O and the mixture extracted with ethyl acetate. The extract is washed with H2O, 1NHCl, 1MNaHCO3 and dried (Na2SO4). The solvent removed under vacuum and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.

Provenance & Evidence