Reaktion #683031
ord-b72c715eb5734b23879523d7ca3a1739
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigethe reaction complete
- 2SonstigeAfter quenched with sat Na2S2O3 and NaHCO3
- 3workup.STIRRINGstirred for 30 min
- 4ExtraktionThe reaction mixture was extracted with EtOAc 3 times
- 5WaschenWashed
- 6SonstigeDried
- 7Einengenconcentrated
- 8SonstigeThe crude material was triturated with ether
- 9Sonstigetaken to the next step without further purification
- 10Sonstige192.9 (MH+), 0.32 min.
Vorschrift
To a solution of 4-fluoropyridin-2-amine (400 mg, 3.57 mmol) in acetonitrile (35. 7 mL) was added NBS (648 mg, 3.64 mmol) in three portions at 0° C. The reaction mixture was stirred at 0° C. for 20 min. LCMS showed the reaction complete. After quenched with sat Na2S2O3 and NaHCO3, stirred for 30 min. The reaction mixture was extracted with EtOAc 3 times. Washed by sat NaHCO3, water and brine. Dried and concentrated. The crude material was triturated with ether and taken to the next step without further purification. LCMS (m/z): 192.9 (MH+), 0.32 min.