反应详情

To a solution of benzaldehyde 4 (0.54 g, 5.05. mmol) in DMF (5 mL) was added compound 1 (2.0 g, 10.1 mmol) and the solution was repeatedly evacuated in a short time to remove oxygen and flushed with Ar, followed by the addition of Cs2CO3 (1.65 g, 5.05 mmol) and the evacuation-flushing process was repeated again. The resultant mixture was stirred for 3.5 h at room temperature. After the solvent was removed by evaporation, the residue was dissolved in the mixture of EtOAc and 10% Na2CO3, and the organic phase was washed with 10% Na2CO3 again and saturated NaCl for three times, dried over Na2SO4 and concentrated in vacuo. The residual solid was recrystalized from MeOH-ether to obtain a off-white solid of 17; yield 1.95 g (79%).

1. customthe solution was repeatedly evacuated in a short time
2. customto remove oxygen
3. customflushed with Ar
4. customAfter the solvent was removed by evaporation
5. dissolutionthe residue was dissolved in the mixture of EtOAc and 10% Na2CO3
6. washthe organic phase was washed with 10% Na2CO3 again
7. dry with materialsaturated NaCl for three times, dried over Na2SO4
8. concentrationconcentrated in vacuo
9. customThe residual solid was recrystalized from MeOH-ether