Reaktion #1846634

ord-1eae9fdaadaa46f7a91def20e14a0b01

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwere charged 62 g
  2. 2
    SonstigeThe autoclave was purged with hydrogen
  3. 3
    Sonstigeat 90° C. to 95° C
  4. 4
    FiltrationThe reaction mixture was filtered through Celite
  5. 5
    Sonstigethe ethanol was evaporated
  6. 6
    workup.DISTILLATIONThe final product was distilled at 93° C. to 98° C./7 to 10 torr
  7. 7
    Sonstigeto yield 47.2 g

Vorschrift

To a 1 liter stirred autoclave were charged 62 g. (0.3 mole) of 2-nitro-1,3-dimethyl-5-tertiary-butyl-benzene, 300 ml. of ethanol and 1.0 g. of 5% palladium on charcoal. The autoclave was purged with hydrogen and then pressure to 1000 psig at 90° C. to 95° C. After 1 hour, the reaction was stopped. A total of 500 psig were taken up. The reaction mixture was filtered through Celite and the ethanol was evaporated. The final product was distilled at 93° C. to 98° C./7 to 10 torr to yield 47.2 g. of a very pale yellow liquid. An 89% isolated yield of 99+% pure 2,6-dimethyl-4-tertiary-butylaniline was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04340758uspto-grants-1982_07