2-Chloropyridin-4-amine → 3-Bromo-2-chloropyridin-4-amine

4-amino-2-chloropyridine (50 g, 388 mmol) was dissolved in glacial acetic acid (500 mL). To this solution was added N-bromosuccinamide (75 g, 426 mmol,) portionwise at room temperature (water bath cooling was provided to control the exothermicity). The reaction mixture was stirred at RT for 1 h at which point the reaction was found complete (as monitored by TLC). Solvent was removed under reduced pressure followed by azeotropic distillation with ethanol. The crude product was purified by column chromatography on silica gel (230-400 mesh) eluting with ethyl acetate hexane mixture.

1. temperaturecooling
2. customwas provided
3. customSolvent was removed under reduced pressure
4. distillationfollowed by azeotropic distillation with ethanol
5. customThe crude product was purified by column chromatography on silica gel (230-400 mesh)
6. washeluting with ethyl acetate hexane mixture

ORD-Eintrag

ord-e0bad5afb81747a7bbc5cfe197c05270

Quelldatensatz

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08524900B2