反应详情

To a solution of (+/−)-4-(6-aminopyridin-3-yl)-1-methylpiperidin-2-one (291 mg, 1.418 mmol) in acetonitrile (14.200 mL) was added NBS (202 mg, 1.134 mmol) at 0° C. The reaction mixture was stirred for 30 min upon warming-up to room temperature. After quenched with Na2S2O3 solution, the reaction mixture was extracted with EtOAc, which was washed with NaHCO3 solution and brine. The organic layer was dried over anhydrous Na2SO4, filtered off, concentrated in vacuo. The crude product (+/−)-4-(6-amino-5-bromopyridin-3-yl)-1-methylpiperidin-2-one (98%) was used for the next step. LCMS (m/z): 284/286 (MH+), 0.34 min.

1. customAfter quenched with Na2S2O3 solution
2. extractionthe reaction mixture was extracted with EtOAc, which
3. washwas washed with NaHCO3 solution and brine
4. dry with materialThe organic layer was dried over anhydrous Na2SO4
5. filtrationfiltered off
6. concentrationconcentrated in vacuo
7. custom284/286 (MH+), 0.34 min.