Reaktion #430450

ord-c1509082ca37431e9befdb5f19a240a9

Reaktionsgleichung

O=[N+]([O-])c1ccccc1CO
2-nitrobenzyl alcohol
CCCCCCCCN=C=O
octyl isocyanate
CCCCCCCCNC(=O)OCc1ccccc1[N+](=O)[O-]
o-nitrobenzyl n-octylcarbamate
Ausbeute 62.1%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturat reflux under nitrogen for 2 hours
  3. 3
    Temperaturcooled
  4. 4
    WaschenThe reaction solution was washed with water several times
  5. 5
    Trocknenthe resulting toluene solution was then dried over sodium sulfate
  6. 6
    FiltrationThe sodium sulfate was filtered off
  7. 7
    Sonstigethe solvent was removed from the filtrate on a rotary evaporator
  8. 8
    SonstigeThe resulting solid was recrystallized twice from hexane

Vorschrift

100 mL toluene, 10 g 2-nitrobenzyl alcohol, and 11.4 g octyl isocyanate were placed in a 200-mL roundbottom flask, heated at reflux under nitrogen for 2 hours, and then cooled. The reaction solution was washed with water several times and the resulting toluene solution was then dried over sodium sulfate. The sodium sulfate was filtered off and the solvent was removed from the filtrate on a rotary evaporator. The resulting solid was recrystallized twice from hexane, yielding 12.5 g o-nitrobenzyl n-octylcarbamate as light yellow needle-like crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05861235uspto-grants-1999_01