Ammonia → HCID 86721459, compound

Participants

Reaction Conditions

Reaction Steps

[step 6] (E)-3-{[11(6H)-(1-cyanoethylidene)-3-fluorodibenzo[b,e]oxepin-8-yl]methyl}-2-cyclopropylimidazo[1,2-a]pyridine-7-carboxylic acid (2.4 g, 5.1 mmol) obtained in step 5 was suspended in THF (25 mL), 1,1′-carbonyldiimidazole (4.1 g, 25 mmol) was added, and the mixture was stirred with heating at 60° C. for 1.5 hr. To the reaction mixture was added 25% aqueous ammonia solution (4.4 mL, 51 mmol), and the mixture was stirred at room temperature for 15 min. To the mixture was added 2 mol/L hydrochloric acid, and the mixture was stirred at room temperature for 1.5 hr. The precipitated crystals were collected by suction filtration, and dried at 50° C. under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform/methanol=100/0 v/v-10/90 v/v) to give the title compound (2.1 g, 86%).

Provenance & Evidence