反应详情

温度

90 °C

To a solution of ethyl-3-aminopyridine-4-carboxylate hydrochloride (1.0 g, 4.93 mmol) and pyridine (1.2 ml, 14.8 mmol) in toluene (10 ml) at room temperature under argon was added 20% phosgene in toluene (3.7 ml, 7.15 mmol) and the mixture was heated at 90° C. for 1 h. The mixture was filtered, and the filtrate was concentrated to dryness. The crude material was dissolved in toluene (10 ml), (5-phenyl-benzofuran-2-yl)-methanol (0.922 g, 4.11 mmol) and DMAP (0.05 g, 0.411 mmol) were added and the mixture was heated at 90° C. for 18 h. The solvent was evaporated to dryness. Purification by chromatography gave 0.538 g of 3-(5-phenyl-benzofuran-2-ylmethoxycarbonylamino)-isonicotinic acid ethyl ester as a white solid.

1. filtrationThe mixture was filtered
2. concentrationthe filtrate was concentrated to dryness
3. dissolutionThe crude material was dissolved in toluene (10 ml)
4. temperaturethe mixture was heated at 90° C. for 18 h
5. customThe solvent was evaporated to dryness
6. customPurification by chromatography