Reaktion #164610

ord-f5e87f5aac9b41b1878c83a473639e46

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeFlask was evacuated
  2. 2
    workup.ADDITIONhydrogen was introduced with the help of balloon
  3. 3
    FiltrationOn completion, the reaction mixture was filtered through celite pad
  4. 4
    SonstigeThe filterate was evaporated

Vorschrift

To a solution of 4-(2,6-difluoro-4-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (Intermediate II) (30 g, 0.09 mol), in methanol (500 mL) under argon atmosphere was added 10% Pd/C (4.5 g, 15 mol% by weight). Flask was evacuated and hydrogen was introduced with the help of balloon. The reaction mixture was stirred under hydrogen and progress of the reaction was monitored by TLC. On completion, the reaction mixture was filtered through celite pad using methanol as solvent. The filterate was evaporated to provide title compound (26 g, 95%) as pale yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841306B2uspto-grants-2014_09