Reacción #529781

ord-a617c26638054dba8697dfdaaf9add5b

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    Temperaturaunder reflux for 1 hour under nitrogen
  3. 3
    TemperaturaAfter cooling
  4. 4
    LavadoThe reaction solution was then washed several times with water
  5. 5
    Secadothe resulting toluene solution was dried over sodium sulfate
  6. 6
    FiltraciónThe sodium sulfate was thereafter filtered off
  7. 7
    Otrothe solvent was eliminated from the filtrate on a rotary evaporator
  8. 8
    OtroThe resulting solid was recrystallized from toluene

Procedimiento

10 mL toluene, 3.1 g 2-nitrobenzyl alcohol, and 2.5 g cyclohexylisocyanate were introduced into a 100-mL three-neck flask and heated under reflux for 1 hour under nitrogen. After cooling, an additional 0.5 g cyclohexylisocyanate was added and the reaction was stirred for 1 hour at ambient temperature. The reaction solution was then washed several times with water and the resulting toluene solution was dried over sodium sulfate. The sodium sulfate was thereafter filtered off and the solvent was eliminated from the filtrate on a rotary evaporator. The resulting solid was recrystallized from toluene to yield ortho-nitrobenzyl cyclohexylcarbamate as light-yellow, needle-like crystals. mp=101°-102° C. Identification by the proton NMR spectrum.

Fuente

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