反应详情

温度

70 °C

3-bromo-6-chloro-2-methoxypyridine (1.15 g, 5.17 mmol), tert-butyl piperazine-1-carboxylate (900 mg, 4.8 mmol), sodium tert-butoxide (1.39 g, 14.5 mmol), Pd2(dba)3 (130 mg, 0.15 mmol) and XantPhos (250 mg, 0.44 mmol) were taken up in toluene (36 mL) under Ar. The reaction mixture was heated to 70° C. and was stirred for 18 h. The mixture was cooled and partitioned between water and EtOAc. The phases were separated, and the organic phase was dried over Na2SO4, filtered, and concentrated. The crude residue was purified by silica gel chromatography (0-3% Et2O in DCM) to afford tert-butyl 4-(6-chloro-2-methoxypyridin-3-yl)piperazine-1-carboxylate 7.10. LCMS-ESI+ (m/z): [M+H]+ calcd for C15H23ClN3O3: 328.1; found: 328.3.

1. temperatureThe mixture was cooled
2. custompartitioned between water and EtOAc
3. customThe phases were separated
4. dry with materialthe organic phase was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude residue was purified by silica gel chromatography (0-3% Et2O in DCM)