Triethylamine → HCID 69054588, compound

Participants

Reaction Steps

To a solution of (2E)-3-{1-[bis(4-fluorophenyl)methyl]-3-cyano-4,6-dimethyl-1H-pyrrolo[2,3-b]pyridin-2-yl}prop-2-enoic acid (200 mg, 0.451 mmol) in THF (2 ml) were added DMF (0.020 ml) and oxalylchloride (0.0471 ml, 0.540 mmol), the mixture was stirred at room temperature for 1 hour and the solvent was distilled off under reduced pressure. The residue was added under ice-cooling to a solution of dimethylbutylamine (121 mg, 0.900 mmol), triethylamine (0.251 ml, 1.80 mmol) and THF (2 ml), and the mixture was stirred under ice-cooling for 2 hours and at room temperature for 12 hours. The reaction solution was poured into water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from hexane and ethyl acetate. Yield (amount) 190 mg, yield (rate) 74.1%

Provenance & Evidence