Phosgene → 2,6-dimethyl-N-butylphenylcarbamoyl chloride

HRID 1447819Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1447819
[CH2:1]([NH:5][C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:13])[CH2:2][CH2:3][CH3:4].[C:14](Cl)([Cl:16])=[O:15]>C1(C)C=CC=CC=1>[CH3:13][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]([CH3:12])[C:6]=1[N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:14]([Cl:16])=[O:15]

Komponenten

4

Edukt 2

HCID 6371PhosgeneHCID 5251001N-butyl-2,6-dimethylaniline

Produkt 1

HCID 544782032,6-dimethyl-N-butylphenylcarbamoyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a suspension of 31.5 g. of N-butyl-2,6-dimethylaniline in 400 ml. of toluene is added 50 ml. of phosgene. The solution is heated to reflux and refluxed for 30 minutes. The solvent is then allowed to distill off (ca 350 ml.) and then cooled. The solution is evaporated in vacuo to a light oil which is then dissolved into hexane, filtered and the hexane evaporated off in vacuo to give a milky oil which is then distilled to give 2,6-dimethyl-N-butylphenylcarbamoyl chloride (b.p. 105° C./0.1 mm)

Aufarbeitung

  1. additionTo a suspension of 31.5 g
  2. temperatureThe solution is heated
  3. temperatureto reflux
  4. temperaturerefluxed for 30 minutes
  5. distillationto distill off (ca 350 ml.)
  6. temperaturecooled
  7. customThe solution is evaporated in vacuo to a light oil which
  8. dissolutionis then dissolved into hexane
  9. filtrationfiltered
  10. customthe hexane evaporated off in vacuo
  11. customto give a milky oil which
  12. distillationis then distilled

Quellen und Nachweise

ORD-Eintrag
ord-75fe104b2a644224a4780d71df67e7bd
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04178387

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