反应详情

温度

122 °C

6-({2-[Allyl-(2-nitro-benzenesulfonyl)-amino]-ethyl}-methanesulfonyl-amino)-2-(4-fluoro-phenyl)-5-iodo-furo[2,3-b]pyridine-3-carboxylic acid methylamide (50 mg, 0.07 mmol) is dissolved in DMF/H2O (10:1, 2 mL: 0.2 mL) and diacetoxypalladium (0.5 mg, 2.64 umol), 1,3-bis(diphenylphosphino)propane (8.17 mg, 0.02 mmol) and potassium carbonate (13.7 mg, 0.10 mmol) are added together then heated in the microwave for 20 min at 122° C. The mixture is then filtered through a bed of celite and the solid is washed with EtOAc (25 mL). The combined organic is then washed with H2O (10 mL), Brine (10 mL) and dried over Na2SO4, followed by evaporation of the solvent. HPLC (CH3CN/H2O/0.1% TFA) provides 2-(4-Fluoro-phenyl)-10-methanesulfonyl-5-methylene-7-(2-nitro-benzenesulfonyl)-5,6,7,8,9,10-hexahydro-1-oxa-7,10,11-triaza-cycloocta[f]indene-3-carboxylic acid methylamide (10 mg, 27%). MS-ES [M+H]+=632.3 and 2-(4-Fluoro-phenyl)-5-iodo-6-{methanesulfonyl-[2-(2-nitro-benzenesulfonylamino)-ethyl]-amino}-furo[2,3-b]pyridine-3-carboxylic acid methylamide (3 mg, 7%). MS-ES [M+H]+=718.0.

1. filtrationThe mixture is then filtered through a bed of celite
2. washthe solid is washed with EtOAc (25 mL)
3. washThe combined organic is then washed with H2O (10 mL), Brine (10 mL)
4. dry with materialdried over Na2SO4
5. customfollowed by evaporation of the solvent