反应详情

A mixture of the nitro compound 50 (890 mg, 2.41 mmol), pyridin-4-ylboronic acid (593 mg, 2 eq, 4.82 mmol), CsF (1.1 g, 3 eq, 7.23 mmol) and Pd(PPh3)4 (278 mg, 0.1 eq, 0.241 mmol) were suspended in DME (30 ml) and NaHCO3 (607 mg, 3 eq, 7.23 mmol), dissolved in the minimum amount of water, was added. The mixture was de-aerated by bubbling N2 through the solution for 10 min, heated to reflux for 4 hrs and concentrated to dryness. The formed residue was dissolved in DCM and washed with water. The DCM was collected, dried over sodium sulfate, filtered and the DCM was removed by evaporation. The resultant solid was triturated with Et2O to afford the title compound 63 (660 mg, 75% yield), which was used without further purification. MS (m/z): 368.0 (M+H).

1. additionwas added
2. customby bubbling N2 through the solution for 10 min
3. temperatureheated
4. temperatureto reflux for 4 hrs
5. concentrationconcentrated to dryness
6. dissolutionThe formed residue was dissolved in DCM
7. washwashed with water
8. customThe DCM was collected
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. customthe DCM was removed by evaporation
12. customThe resultant solid was triturated with Et2O