Potassium Fluoride → 2-Chloro-4,5-difluorobenzonitrile

HRID 1729485

Reaktionsgleichung

Reaktionsgleichung von HRID 1729485
[Cl:1][C:2]1[CH:9]=[C:8](Cl)[C:7]([F:11])=[CH:6][C:3]=1[C:4]#[N:5].[F-:12].[K+]>CS(C)=O>[Cl:1][C:2]1[CH:9]=[C:8]([F:12])[C:7]([F:11])=[CH:6][C:3]=1[C:4]#[N:5]

Komponenten

4

Edukt 2

HCID 522689Potassium FluorideHCID 27827532,4-Dichloro-5-fluorobenzonitrile

Produkt 1

HCID 40858492-Chloro-4,5-difluorobenzonitrileAusbeute 68,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

A mixture comprising 5.70 g (0.03 mol) of 2,4-dichloro-5-fluorobenzonitrile, 3.48 g (0.06 mol) of spray dried KF and 30 ml of dimethylsulfoxide, was reacted at a temperature of from 140° to 150° C. for 3.5 hours in a glass reactor. After completion of the reaction, the mixture was poured into ice water (50 ml) and extracted with chloroform. The chloroform extract was washed five times with water and then dried. Then chloroform was distilled off. The residue was distilled under reduced pressure to obtain 3.57 g (yield: 68.6%) of 2-chloro-4,5-difluorobenzonitrile. Boiling point: 105°-107° C./37 mmHg; melting point: 35°-37° C.

Aufarbeitung

  1. customAfter completion of the reaction
  2. extractionextracted with chloroform
  3. extractionThe chloroform extract
  4. washwas washed five times with water
  5. customdried
  6. distillationThen chloroform was distilled off
  7. distillationThe residue was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6bc9dc00baca4272a4c1fb4f5e1ef79e
Quelldatensatz
uspto-grants-1994_07
Patentnummer
US05332851

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