反应详情

A mixture of {[2-(trifluoromethyl)-1H-indol-5-yl]methyl}amine hydrochloride (Intermediate 5, 1 g, 3.99 mmol), 6-bromo-3-pyridinecarboxylic acid (Matrix Scientific; 0.887 g, 4.39 mmol), EDC (0.841 g, 4.39 mmol), HOBT (0.672 g, 4.39 mmol) and DIPEA (2.8 ml, 16.03 mmol) in DCM (50 ml) was stirred at room temperature for 18 hrs. The mixture was stirred well with saturated aqueous NaHCO3 solution, the organics separated and the aqueous further extracted (EtOAC×3). The combined organics were dried (Phase-Sep cartridge) and evaporated under reduced pressure to a white solid. Trituration with diethyl ether overnight and filtration afforded a crude white solid (1.16 g). A portion (88 mg) was further purified via MDAP to afford the title compound as a white solid (54 mg);

1. customthe organics separated
2. extractionthe aqueous further extracted (EtOAC×3)
3. customThe combined organics were dried (Phase-Sep cartridge)
4. customevaporated under reduced pressure to a white solid
5. filtrationTrituration with diethyl ether overnight and filtration
6. customafforded a crude white solid (1.16 g)
7. customA portion (88 mg) was further purified via MDAP