反应详情

To a stirred mixture of 1-(4-fluoro-phenyl)-1H-pyrazolo[3,4-c]pyridine-4-carboxylic acid (0.310 g, 1.21 mmol), N,N-diisopropylethylamine (0.630 mL, 3.62 mmol) and 1-(5-methanesulfonyl-furan-2-yl)-cyclopropylamine-hydrochloride salt (364 mg, 1.53 mmol) in DMF (30 mL) is added (benzotriazol-1-yloxy)tripyrrolidinophosphonium hexafluorophosphate (PyBOP) (0.650 g, 1.25 mmol). After 18 hours, the mixture is diluted with saturated aqueous ammonium chloride (100 mL) and extracted with ethyl acetate (4×30 mL). The combined organic layers are washed with brine (50 mL), dried over sodium sulfate, filtered and concentrated. The residue is purified by silica gel chromatography eluting with a gradient of 0-100% ethyl acetate in hexanes to afford the title compound as a solid.

1. extractionextracted with ethyl acetate (4×30 mL)
2. washThe combined organic layers are washed with brine (50 mL)
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is purified by silica gel chromatography
7. washeluting with a gradient of 0-100% ethyl acetate in hexanes