反应详情

To a mixture of the nitro compound 50 (440 mg, 1.19 mmol) in DME (20 ml) was added the boronate 75 (667 mg, 1.5 eq, 1.79 mmol), CsF (542 mg, 3 eq, 3.57 mmol) and Pd(PPh3)4 (139 mg, 0.1 eq, 0.19 mmol) were suspended in DME (30 ml) and NaHCO3 (100 mg, 3 eq, 3.57 mmol), dissolved in the minimum amount of water, was added. The mixture was deaerated by bubbling N2 through the solution for 10 min, heated to reflux for 4 hrs. The mixture was cooled to room temperature, diluted with EtOAc and water then the organic phase was collected, dried over sodium sulfate and filtered. The solvent was removed and the residue was purified by column chromatography (20% MeOH in EtOAc+1% TEA) to afford title compound 79 as brown oil (248 mg, 39% yield). MS (m/z): 536.1 (M+H).

1. additionwas added
2. customby bubbling N2 through the solution for 10 min
3. temperatureheated
4. temperatureto reflux for 4 hrs
5. additiondiluted with EtOAc and water
6. customthe organic phase was collected
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customThe solvent was removed
10. customthe residue was purified by column chromatography (20% MeOH in EtOAc+1% TEA)