反应详情

Add tetrakistriphenylphosphine palladium(0)(0.01 g, 0.01 mmol) to 1′-(5-iodo-1H-benzimidazol-2-yl)-spiro[isobenzofuran-1,4′-piperidin]-3-one (0.10 g, 0.22 mmol) in ethylene glycol dimethyl ether (2 mL). To this solution, add pyridine-3-boronic acid (0.06 g, 0.45 mmol) and aqueous sodium carbonate (1M, 1 mL) and heat the reaction at 80° C. for 2 hours. Extract the product with EtOAc (20 mL). Wash the combined extracts with brine (20 mL), dry over sodium sulfate, and concentrate in vacuo. Purify by flash column chromatography (5% MeOH—CH2Cl2) to obtain 1′-(5-pyridin-3-yl-1H-benzimidazol-2-yl)-spiro[isobenzofuran-1,4′-piperidin]-3-one as a white solid.

1. temperatureheat
2. customthe reaction at 80° C. for 2 hours
3. extractionExtract the product with EtOAc (20 mL)
4. washWash the combined extracts with brine (20 mL)
5. dry with materialdry over sodium sulfate
6. concentrationconcentrate in vacuo
7. customPurify by flash column chromatography (5% MeOH—CH2Cl2)