Reaktion #1176591

ord-1858b73381794dca9195d2912187317d

Reaktionsgleichung

CCCCC(CC)CN
2-ethylhexylamine
COC(N)=O
methyl carbamate
Cc1ccccc1
toluene
CCCCC(CC)CNC(N)=O
N-(2-ethylhexyl)urea
Ausbeute 91.7%

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeInto a 300 ml reaction vessel
  2. 2
    Temperaturheated
  3. 3
    Sonstigewas removed
  4. 4
    Temperaturthe mixture was refluxed
  5. 5
    Temperaturby heating for 30 minutes
  6. 6
    workup.STIRRINGwith stirring
  7. 7
    Temperaturto cool
  8. 8
    workup.DISTILLATIONThe toluene was distilled off under reduced pressure
  9. 9
    Waschenthe residue was washed with n-hexane
  10. 10
    Filtrationcollected by filtration

Vorschrift

Into a 300 ml reaction vessel equipped with a distillation apparatus, 50 g of 2-ethylhexylamine, 29 g of methyl carbamate and 100 ml of toluene were placed, and to the mixture was added 0.1 g of dibutyl tin oxide as a catalyst and heated with stirring. Methanol formed during the reaction was removed, when the reflux temperature was raised to 110° C., i.e.,the boiling point of toluene, the distillation apparatus was taken off and instead a reflux condenser was attached and the mixture was refluxed by heating for 30 minutes with stirring, then allowed to cool. The toluene was distilled off under reduced pressure, and the residue was washed with n-hexane and collected by filtration to obtain 61 g of N-(2-ethylhexyl)urea.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04966835uspto-grants-1990_10