Reaktion #50004

ord-599d75b7d02443e5b36146fca1375b02

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated for 5 hours
  2. 2
    Temperaturunder reflux
  3. 3
    TemperaturAfter cooling
  4. 4
    Sonstigethe solvent was removed in vacuo
  5. 5
    Sonstigethe residue recrystallised several times from ethyl acetate

Vorschrift

2.6 g Ethyl piperidine-2-carboxylate was added to a solution of 4.2 g 2,4-dichloro-6-fluoro-7-isocyanato-benzothiazole in 50 ml tetrahydrofuran. The mixture was heated for 5 hours under reflux. After cooling, the solvent was removed in vacuo and the residue recrystallised several times from ethyl acetate. Yield: 2.5 g=42% of theory m.p.: 168°-170° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424443uspto-grants-1995_06