5-Fluoro-2-(2,2,2-trifluoroethoxy)nitrobenzene → 5-Fluoro-2-(2,2,2-trifluoroethoxy)aniline

HRID 2185920Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2185920
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[C:6]([N+:8]([O-])=O)[CH:7]=1>C(OCC)(=O)C.[Ni]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:12][C:13]([F:14])([F:15])[F:16])=[C:6]([CH:7]=1)[NH2:8]

Komponenten

4

Edukt 1

HCID 234479215-Fluoro-2-(2,2,2-trifluoroethoxy)nitrobenzene

Produkt 1

HCID 174854135-Fluoro-2-(2,2,2-trifluoroethoxy)anilineAusbeute 90,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
22.5 °C

Versuchsvorschrift

A mixture of 0.66 g of Compound 8A and 0.07 g of Raney-Nickel in 20 mL of ethyl acetate was stirred for 14 hours at 20-25° C. The catalyst was filtered off. The mixture was diluted with water. The organic layer was separated and the mixture extracted with 2×40 mL of ethyl acetate. The combined organic layers were washed with 20 mL of brine, dried over sodium sulphate and evaporated to dryness in vacuo to afford 0.52 g (90.6%) of Compound 8B as an oil.

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. additionThe mixture was diluted with water
  3. customThe organic layer was separated
  4. extractionthe mixture extracted with 2×40 mL of ethyl acetate
  5. washThe combined organic layers were washed with 20 mL of brine
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e59feff57bef42659ba9126a19a4b812
Quelldatensatz
uspto-grants-2002_06
Patentnummer
US06403594B1

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