2,6-Dimethylphenol → 2,4,5-Trifluoro-6-(2,6-xylyloxy)isophthalonitrile

HRID 65454

Reaktionsgleichung

Reaktionsgleichung von HRID 65454
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[OH:9].F[C:11]1[C:16]([C:17]#[N:18])=[C:15]([F:19])[C:14]([C:20]#[N:21])=[C:13]([F:22])[C:12]=1[F:23].[F-].[K+]>C(#N)C.CC(C)=O.C1CCCCC1>[F:19][C:15]1[C:14]([C:20]#[N:21])=[C:13]([F:22])[C:12]([F:23])=[C:11]([O:9][C:3]2[C:4]([CH3:8])=[CH:5][CH:6]=[CH:7][C:2]=2[CH3:1])[C:16]=1[C:17]#[N:18]

Komponenten

7

Edukt 3

HCID 113352,6-DimethylphenolHCID 522689Potassium FluorideHCID 608182Tetrafluoroisophthalonitrile

Produkt 1

HCID 136561882,4,5-Trifluoro-6-(2,6-xylyloxy)isophthalonitrileAusbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 180AcetoneLösungsmittelHCID 6342AcetonitrileLösungsmittelHCID 8078CyclohexaneLösungsmittel

Versuchsvorschrift

A solution of 1.2 g (10×10-3 mol) of 2,6-dimethylphenol in 40 ml of acetonitrile was dropwise added at a temperature of -10° C. to a solution of 2.0 g (10×10-3 mol) of tetrafluoroisophthalonitrile and 2.9 g (50×10-3 mol) of potassium fluoride. The mixture was allowed to stand at a temperature of -10° C. to 0° C. for 1 hour while stirring and the undissolved potassium fluoride was separated by filtration. The filtrate was concentrated to dryness in vacuo. The resultant residue was dissolved in a mixed solvent of acetone and cyclohexane and 2.3 g (77% yield) of the desired compound No. 37 was obtained as white crystal.

Aufarbeitung

  1. customthe undissolved potassium fluoride was separated by filtration
  2. concentrationThe filtrate was concentrated to dryness in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9472bc0a7bf046da91c69ec8bf50cbce
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04614742

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