反应详情

A solution of 5-(3-cyanopropyl)-N-cyclopropyl-1-{4-[(ethylamino)carbonyl]phenyl}-1H-1,2,3-triazole-4-carboxamide (183 mg, 0.5 mmol) obtained in Example 1207, trimethylsilyl azide (58 mg, 0.5 mmol) and di-N-butyltin oxide (12.5 mg, 0.05 mmol) in toluene (5 ml) was boiled under reflux for 24 hr and the solvent was evaporated. Methanol (5 ml) was added to the residue, and the solvent was evaporated again. Ethyl acetate (10 ml) and 6% aqueous sodium bicarbonate solution (10 ml) were added to the residue and, after partitioning, the aqueous layer was adjusted to pH 4-5 with 1N hydrochloric acid, and the precipitated crystals were collected by filtration and dried to give the title compound as a colorless powder (55 mg, 27%).

1. temperatureunder reflux for 24 hr
2. customthe solvent was evaporated
3. additionMethanol (5 ml) was added to the residue
4. customthe solvent was evaporated again
5. additionEthyl acetate (10 ml) and 6% aqueous sodium bicarbonate solution (10 ml) were added to the residue
6. customafter partitioning
7. filtrationthe precipitated crystals were collected by filtration
8. customdried