Reaktion #84899

ord-d64eab8bf2004c5f897bd6daf3c9a8ec

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was then filtered through Celite
  2. 2
    Einengenthe filtrate was concentrated under reduced pressure
  3. 3
    Sonstigedried
  4. 4
    SonstigeThe crude product was purified by normal phase chromatography (mobile phase: cyclohexane/ethyl acetate 15%-20% mixtures)

Vorschrift

A solution of 1000 mg (2.82 mmol) of tert-butyl 2,5-difluoro-4-nitrobenzoate in 8 ml of tetrahydrofuran and 8 ml of ethyl acetate was hydrogenated in the presence of 65.6 mg of palladium (10% on activated carbon) at RT and standard pressure. The reaction mixture was then filtered through Celite and the filtrate was concentrated under reduced pressure and dried. The crude product was purified by normal phase chromatography (mobile phase: cyclohexane/ethyl acetate 15%-20% mixtures). Yield: 155 mg (purity 85%, 20% of theory)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434690B2uspto-grants-2016_09