Reaktion #486554

Reaktionsgleichung

2-nitrobenzyl alcohol

benzyl isocyanate

→

o-nitrobenzyl benzylcarbamate

Ausbeute 67.9%

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle