反应详情

To a solution of N-(5-chloropyridin-2-yl)-2-amino-benzamide (0.247 g, 1 mmol) in dichloromethane (10 mL) and pyridine (0.5 mL) was added a solution of 4-biphenylcarbonyl chloride (0.217 g, 1 mmol) in dichloromethane (5 mL). After stirring overnight the solvent was removed in vacuo. The residue was partitioned between ethyl acetate (50 mL) and water (25 mL). Separate the layers and wash the organic layer with water (2×10 mL), saturated sodium bicarbonate (2×20 mL), hydrochloric acid (0.2 N, 1×20 mL). Dried over MgSO4, filtered and concentrated in vacuo. The residue was then purified by RPHPLC (30% ethyl acetate/hexane) to give 0.4 g (94%) of pure product.

1. customwas removed in vacuo
2. customThe residue was partitioned between ethyl acetate (50 mL) and water (25 mL)
3. customSeparate the layers
4. washwash the organic layer with water (2×10 mL), saturated sodium bicarbonate (2×20 mL), hydrochloric acid (0.2 N, 1×20 mL)
5. dry with materialDried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was then purified by RPHPLC (30% ethyl acetate/hexane)