反应详情

温度

90 °C

To a solution of 5-amino-biphenyl-3-carboxylic acid methyl ester (crude from Step 4; 1.00 g, 4.40 mmol) and pyridine (0.711 mL, 8.80 mmol) in toluene (15 mL) at room temperature under argon was added 20% phosgene in toluene (3.3 mL, 6.3 mmol) and the mixture was heated at 90° C. for 1 h. The mixture was filtered, and the filtrate was concentrated to dryness (0.373 g). The crude material was dissolved in toluene (4 mL), (5-phenyl-benzofuran-2-yl)-methanol (0.300 g, 1.38 mmol) and DMAP (0.016 g, 0.137 mmol) were added and the mixture was heated at 90° C. for 18 h. The solvent was evaporated to dryness. Purification by flash chromatography gave 0.125 g of a white solid.

1. filtrationThe mixture was filtered
2. concentrationthe filtrate was concentrated to dryness (0.373 g)
3. dissolutionThe crude material was dissolved in toluene (4 mL)
4. temperaturethe mixture was heated at 90° C. for 18 h
5. customThe solvent was evaporated to dryness
6. customPurification by flash chromatography