Reaktion #5853

ord-8640071052634bebb681ae075425f7b2

Reaktionsgleichung

CC(C)c1cccc(C(C)C)c1NC(=N)Nc1c(C(C)C)cccc1C(C)C
N,N'-bis-(2,6-diisopropylphenyl) guanidine
Cc1cccc(C(Cl)Cl)c1
α,α-dichloro-m-xylene
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC(C)c1cccc(C(C)C)c1NC(=NCc1cccc(CCl)c1)Nc1c(C(C)C)cccc1C(C)C
white powder
Ausbeute 32.8%
CC(C)c1cccc(C(C)C)c1NC(=NCc1cccc(CCl)c1)Nc1c(C(C)C)cccc1C(C)C
N,N'-bis-(2,6-diisopropylphenyl)-N"-(3-chloromethylphenyl) methylguanidine
Ausbeute 32.8%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe thus-formed mixture was then refluxed
  2. 2
    Temperaturunder heating for 10 hours
  3. 3
    Temperaturto cool
  4. 4
    Sonstigethe insoluble substance was removed by filtration
  5. 5
    WaschenThe thus-obtained filtrate was washed with water
  6. 6
    Einengenconcentrated for the purpose
  7. 7
    Sonstigeof recovering the solvent and unreacted raw materials
  8. 8
    Sonstigeto obtain a slightly yellow crystal
  9. 9
    SonstigeThe crystal was then recrystallized from acetone

Vorschrift

11.4 g (0.03 mole) of N,N'-bis-(2,6-diisopropylphenyl) guanidine, 5.7 g (0.033 mole) of α,α-dichloro-m-xylene and 2.1 g (0.015 mole) of anhydrous potassium carbonate were added to 50 ml of xylene. The thus-formed mixture was then refluxed under heating for 10 hours. After the mixture had been allowed to cool, the insoluble substance was removed by filtration. The thus-obtained filtrate was washed with water and then concentrated for the purpose of recovering the solvent and unreacted raw materials to obtain a slightly yellow crystal. The crystal was then recrystallized from acetone to obtain 5.1 g of white powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05246810uspto-grants-1993_09