Reacción #486554

Ecuación de reacción

2-nitrobenzyl alcohol

benzyl isocyanate

→

o-nitrobenzyl benzylcarbamate

Rendimiento 67.9%

Disolventes

toluene

toluene

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturato reflux for 3 hours in a nitrogen atmosphere
2. 2
   workup.ADDITIONwas added
3. 3
   LavadoThis reaction solution was washed several times with water
4. 4
   FiltraciónThe sodium sulfate was then filtered out
5. 5
   Otrothe solvent was removed from the filtrate by means of a rotary evaporator
6. 6
   OtroThe solid obtained
7. 7
   Otrowas recrystallized from a hexane-toluene mixed solvent

Procedimiento

10 ml of toluene, 5.75 g of 2-nitrobenzyl alcohol and 5 g of benzyl isocyanate were heated to reflux for 3 hours in a nitrogen atmosphere. Following cooling of the mixture, 50 ml of toluene was added. This reaction solution was washed several times with water, and was then dehydrated with sodium sulfate. The sodium sulfate was then filtered out, and the solvent was removed from the filtrate by means of a rotary evaporator. The solid obtained was recrystallized from a hexane-toluene mixed solvent, producing 7.3 g of o-nitrobenzyl benzylcarbamate in the form of plate yellow crystals. This compound had a melting point of 110° to 111° C., and the infrared absorption spectrum was 3308 cm-1 : N--H, 1696 cm-1 : C=O, 1520 cm-1 : N--O.

Fuente