Reaktion #59079

ord-268b0d3cd39b4da6b661c20374790de7

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    SonstigeReaction
  2. 2
    Einengenthen concentrated
  3. 3
    Sonstigepartitioned between ethyl acetate and water
  4. 4
    TrocknenOrganic layer dried over sodium sulfate and sodium bicarbonate
  5. 5
    Einengenconcentrated

Vorschrift

The mixture containing 4-chloro-3-(3-fluoropyridin-4-yl)benzenamine (1 eq) and sodium bicarbonate (2 eq) in acetone was treated with thiophosgene (2 eq) and stirred for 5 minutes at 0° C. Reaction then concentrated and partitioned between ethyl acetate and water. Organic layer dried over sodium sulfate and sodium bicarbonate and concentrated to give 4-(2-chloro-5-isothiocyanatophenyl)-3-fluoropyridine. HPLC=5.54 min; MS: MH+=265.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423150B2uspto-grants-2008_09