反应详情

To a solution of 3,5-dibromopyridine (Sigma-Aldrich, St. Louis, USA) (1 eq, 8.4 mmol, 2.0 g) and 1-methylpiperazine (Sigma-Aldrich, St. Louis, USA) (1 eq, 8.4 mmol, 0.94 ml) in toluene (20 ml), Pd2(dba)3 (0.02 eq, 0.167 mmol, 153 mg), Xantphos (0.06 eq, 0.50 mmol, 290 mg), and NaOtBu (1.5 eq, 12.5 mmol, 1.2 g) are added. The resulting mixture is heated using microwave radiation at 120° C. for 15 min. The solvents are evaporated and aqueous HCl solution (1 M) is added. The aqueous layer is washed with DCM, adjusted to pH 10, and extracted with DCM. The organic layer is dried, filtered, and concentrated to give the title compound, [M+H]+=257.

1. temperatureThe resulting mixture is heated
2. customat 120° C.
3. customfor 15 min
4. customThe solvents are evaporated
5. additionaqueous HCl solution (1 M) is added
6. washThe aqueous layer is washed with DCM
7. extractionextracted with DCM
8. customThe organic layer is dried
9. filtrationfiltered
10. concentrationconcentrated