Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate

HRID 26536

Reaktionsgleichung

Reaktionsgleichung von HRID 26536
C(Cl)(=O)[C:2](Cl)=[O:3].[F:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:9]=1[C:10]([NH2:12])=[O:11]>ClCCCl>[F:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:9]=1[C:10]([N:12]=[C:2]=[O:3])=[O:11]

Komponenten

4

Edukt 2

HCID 65578Oxalyl chlorideHCID 874392,6-Difluorobenzamide

Produkt 1

HCID 27333692,6-Difluorobenzoyl isocyanate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

Oxalyl chloride (5.5 g) was added slowly to a suspension of 2,6-difluorobenzamide (6.0 g) in 1,2-dichloroethane maintained at a temperature within the range -10° to -5° C. When the addition was complete the mixture was allowed to warm to the ambient temperature, and then gradually heated to the reflux temperature and maintained thereat for a period of 16 hours. The solvent was then removed by evaporation under reduced pressure and the residual oil purified by distillation to yield 2,6-difluorobenzoyl isocyanate, b.p. 60°-61°/0.7 mm.

Aufarbeitung

  1. temperaturemaintained at a temperature within the range -10° to -5° C
  2. additionWhen the addition
  3. temperaturegradually heated to the reflux temperature
  4. temperaturemaintained
  5. customThe solvent was then removed by evaporation under reduced pressure
  6. distillationthe residual oil purified by distillation

Quellen und Nachweise

ORD-Eintrag
ord-f779bab063b2461595cd6647fbefa252
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04150158

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