Reaktion #683031

ord-b72c715eb5734b23879523d7ca3a1739

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe reaction complete
  2. 2
    SonstigeAfter quenched with sat Na2S2O3 and NaHCO3
  3. 3
    workup.STIRRINGstirred for 30 min
  4. 4
    ExtraktionThe reaction mixture was extracted with EtOAc 3 times
  5. 5
    WaschenWashed
  6. 6
    SonstigeDried
  7. 7
    Einengenconcentrated
  8. 8
    SonstigeThe crude material was triturated with ether
  9. 9
    Sonstigetaken to the next step without further purification
  10. 10
    Sonstige192.9 (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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09242996B2uspto-grants-2016_01