反应详情

温度

120 °C

To 5-iodo-N-methyl-6-(methylsulfonamido)-2-(p-tolyl)furo[2,3-b]pyridine-3-carboxamide (crude ˜20%) (400 mg, 0.824 mmol) was added 1,4-dibromobutane (1780 mg, 8.24 mmol) and CESIUM CARBONATE (537 mg, 1.648 mmol) and DMF (4 ml) Heated at 120° C. 30 min. Added water and extracted with EtOAc. Conc. on vac to oil. Added 3 mL ACN and 1 mL water. Filtered with 0.45p filter Purified via HPLC C8 40-80% ACN/H2O (0.1% NH4OH) 40 mL/min over 10 min. to give 6-(N-(4-bromobutyl)methylsulfonamido)-5-iodo-N-methyl-2-(p-tolyl)furo[2,3-b]pyridine-3-carboxamide

1. custom30 min
2. extractionAdded water and extracted with EtOAc
3. additionAdded 3 mL ACN and 1 mL water
4. filtrationFiltered with 0.45p
5. filtrationfilter
6. customPurified via HPLC C8 40-80% ACN/H2O (0.1% NH4OH) 40 mL/min over 10 min.