反应详情

To a mixture of tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate (5 g, 8.65 mmol) in DMF (15 mL) was added N-iodosuccinimide (1.86 g, 8.27 mmol) and the resulting mixture was allowed to stir at room temperature for 1 hour. The mixture diluted with EtOAc (100 mL), washed with water (20 mL). The aqueous layer was extracted with EtOAc (20 mL) once, and combined organic layer was washed with water (20 mL) three times, brine once and dried (MgSO4). After concentration, the residue was purified by column chromatography on silica gel. Elution with EtOAc/Hex (0-30%) gave tert-butyl 4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-3-iodopyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1-carboxylate (4.55 g, 75%). (Note: DMF could be replaced by acetonitrile.)

1. washwashed with water (20 mL)
2. extractionThe aqueous layer was extracted with EtOAc (20 mL) once
3. washwas washed with water (20 mL) three times, brine once
4. dry with materialdried (MgSO4)
5. concentrationAfter concentration
6. customthe residue was purified by column chromatography on silica gel
7. washElution with EtOAc/Hex (0-30%)