反应详情

A mixture of 2-(5-chloro-1H-pyrrolo[2,3-b]pyridin-3-yl)ethanamine hydrochloride (0.070 g; 0.301 mmol), 4-(3-fluorobenzyl)benzoic acid (0.0701 g; 0.304 mmol), HATU (0.116 g: 0.304 mmol) and N,N-diisopropylethylamine (0.132 mL; 0.754 mmol) in DMF (3 mL) was stirred during the weekend at room temperature and was concentrated in vacuo. The residue was dissolved in dichloromethane and the organic layer was washed with water, and concentrated under reduced pressure. The crude material was purified by flash chromatography on silica gel (eluent 0 to 35% of ethyl acetate in dichloromethane) to give 0.061 g (49%) of N-(2-(5-chloro-1H-pyrrolo[2,3-b]pyridin-3-yl)ethyl)-5-(2,5-difluorobenzyl)isoxazole-3-carboxamide as a white solid.

1. concentrationwas concentrated in vacuo
2. dissolutionThe residue was dissolved in dichloromethane
3. washthe organic layer was washed with water
4. concentrationconcentrated under reduced pressure
5. customThe crude material was purified by flash chromatography on silica gel (eluent 0 to 35% of ethyl acetate in dichloromethane)