Reacción #529780

ord-19864d38ed5b4455a9b50cb899a1c02f

Reactivos

Ninguno

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    Temperaturaunder reflux for 2 hours under a nitrogen blanket
  3. 3
    TemperaturaAfter cooling
  4. 4
    Lavadothe reaction solution was washed several times with water
  5. 5
    Otrothe toluene solution thereby afforded
  6. 6
    Secadowas then dried over sodium sulfate
  7. 7
    FiltraciónThe sodium sulfate was thereafter filtered off
  8. 8
    Otroa rotary evaporator
  9. 9
    OtroThe resulting solid was recrystallized twice from hexane

Procedimiento

100 mL toluene, 10 g 2-nitrobenzyl alcohol and 11.4 mL octyl isocyanate were introduced into a 200-mL roundbottom flask and heated under reflux for 2 hours under a nitrogen blanket. After cooling, the reaction solution was washed several times with water, and the toluene solution thereby afforded was then dried over sodium sulfate. The sodium sulfate was thereafter filtered off and the solvent was eliminated from the filtrate using a rotary evaporator. The resulting solid was recrystallized twice from hexane to yield 12.5 g ortho-nitrobenzyl n-octylcarbamate as light-yellow, needle-like crystals. mp=70°-71° C. Infrared absorption=3331 cm-1, 1691 cm-1.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05891529uspto-grants-1999_04