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

HRID 840116Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 840116
[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 5A and 0.07 g of Raney-Nickel in 20 mL of ethyl acetate was stirred for 14 hours at 20-25° C. 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 5B as an orange oil.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-705cd02635274f24bc3d55e2914839f2
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06365591B1

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