反应详情

2-(4-Fluoro-phenyl)-5-iodo-6-methanesulfonylamino-furo[2,3-b]pyridine-3-carboxylic acid methylamide (162 mg, 0.331 mmol), 1-iodo-3-(methylsulfonyl)propane (82 mg, 0.331 mmol) and cesium carbonate (119 mg, 0.364 mmol) in DMF (1656 μL) are heated for 20 min at 150° C. by microwave. 3:1 Product/starting material. An additional 45 mg of alky iodide are added and 60 mg of cesium carbonate and heated for 20 min at 150° C. by microwave. LCMS indicates complete consumption of starting material. Acetonitrile and water are added and the mixture is filtered with 0.45μ PTFE filter. Purification is achieved by reverse phase HPLC with a C8 column with 20-50% ACN//H2O (0.1% NH4OH) over 20 min. Elutes at 13-15 minutes to give the title compound (107 mg, 53%). MS (ESI) m/z 610.0 (M+1). Retention time=1.40 min, Method A.

1. customconsumption of starting material
2. additionAcetonitrile and water are added
3. filtrationthe mixture is filtered with 0.45μ PTFE
4. filtrationfilter
5. customPurification