Reaktion #85834

ord-6887a601b8754e1a9c97c2337c0ce88c

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with EA (3×25 mL)
  2. 2
    Waschenwashed with H2O (25 mL) and brine (25 mL)
  3. 3
    Trocknendried over Na2SO4
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigeto give yellow solid

Vorschrift

To a solution of tert-butyl piperazine-1-carboxylate (1120 mg, 6 mmol) in DMF (25 mL) was added K2CO3 (828 mg, 6 mmol) and 1,2-difluoro-4-nitrobenzene (795 mg, 5 mmol) at room temperature. The reaction was stirred at 80° C. for 24 hours. After that, the reaction was poured into 50 mL of water and extracted with EA (3×25 mL), washed with H2O (25 mL) and brine (25 mL), dried over Na2SO4 and concentrated to give yellow solid. MS (m/z): 226 (M−99)+

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434726B2uspto-grants-2016_09