反应详情

温度

110 °C

To a solution of 6-fluoro-7-iodo-1H-pyrazolo[4,3-b]pyridine (150 mg, 0.570 mmol) in DMF (4 mL) was added Cs2CO3 (279 mg, 0.855 mmol) and tert-butyl 2-chloroacetylcarbamate (121 mg, 0.627 mmol). The mixture was heated at 110° C. for 2 hours. The mixture was then cooled and the reaction was concentrated under vacuum to give a residue. The residue was partitioned between saturated sodium bicarbonate solution and EtOAc (25 mL). The organic layer was separated and the aqueous layer was extracted with EtOAc (25 mL). The combined organic layers were, dried over Na2SO4 and evaporated to give tert-butyl 2-(6-fluoro-7-iodo-2H-pyrazolo[4,3-b]pyridin-2-yl)acetylcarbamate. MS [M+H] found 421.2.

1. temperatureThe mixture was then cooled
2. concentrationthe reaction was concentrated under vacuum
3. customto give a residue
4. customThe residue was partitioned between saturated sodium bicarbonate solution and EtOAc (25 mL)
5. customThe organic layer was separated
6. extractionthe aqueous layer was extracted with EtOAc (25 mL)
7. dry with materialdried over Na2SO4
8. customevaporated