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Water → 3,5-Bis-(2-trifluoromethylpyridin-4-yloxy)benzonitrile

HRID 353205
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 353205
F[C:2]1[CH:3]=[C:4]([CH:7]=[C:8](F)[CH:9]=1)[C:5]#[N:6].[C:11](=[O:14])([O-])[O-].[K+].[K+].[F:17][C:18]([F:27])([F:26])[C:19]1[CH:24]=[C:23]([OH:25])[CH:22]=[CH:21][N:20]=1.O>CN(C)C(=O)C.C(OCC)(=O)C.CCCCCCC>[F:27][C:18]([F:17])([F:26])[C:19]1[CH:24]=[C:23]([O:25][C:2]2[CH:3]=[C:4]([CH:7]=[C:8]([O:14][C:11]3[CH:22]=[CH:21][N:20]=[C:19]([C:18]([F:27])([F:26])[F:17])[CH:24]=3)[CH:9]=2)[C:5]#[N:6])[CH:22]=[CH:21][N:20]=1
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Komponenten

7

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 5872043,5-DifluorobenzonitrileHCID 178516505HCID 178516505, Verbindung

Produkt 1

HCID 115609193,5-Bis-(2-trifluoromethylpyridin-4-yloxy)benzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 31374
Dimethylacetamide
Lösungsmittel
HCID 21899848Ethylacetate heptaneLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

Under an atmosphere of nitrogen, 0.556 g (4.0 mmol) of 3,5-difluorobenzonitrile was initially charged in 10 ml of N,N-dimethylacetamide, and 1.22 g (8.8 mmol) of potassium carbonate were added a little at a time at room temperature. 1.305 g (8.00 mmol) of 2-(trifluoromethyl)pyridin-4-ol were then added and the mixture was heated at 150° C. for 30 h and cooled to room temperature, water and ethyl acetate/heptane (1:1) were added to the reaction solution and the solution was stirred for a number of minutes. The phases were separated and the organic phase was washed repeatedly with water and finally with saturated sodium chloride solution and then dried over sodium sulfate, filtered and concentrated. HPLC of the crude product gave 3,5-bis-(2-trifluoromethylpyridin-4-yloxy)benzonitrile in the form of white crystals.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. customThe phases were separated
  3. washthe organic phase was washed repeatedly with water and finally with saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-8bd2a47560894c11a47af83b98b5e951
Quelldatensatz
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06750222B2

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