Reaktion #93228

Reaktionsgleichung

methyl isocyanate

4-aminophenol

→

N-(4-hydroxyphenyl)-N'-methylurea

Ausbeute 51.8%

Lösungsmittel

acetonitrile

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated under reduced pressure
2. 2
   workup.ADDITIONWater (100 ml) was added to the resulting syrup
3. 3
   workup.STIRRINGthe mixture was stirred for 30 minutes
4. 4
   workup.STIRRINGof stirring
5. 5
   FiltrationThe solid substance was collected by filtration
6. 6
   Waschenwashed with cold water
7. 7
   Sonstigerecrystallized from aqueous alcohol

Vorschrift

A solution of methyl isocyanate (6 g) in acetonitrile (10 ml) was added dropwise to a solution of 4-aminophenol (10.9 g) in N,N-dimethylformamide (50 ml) at 10° C. to 20° C. The mixture was stirred at 25° C. to 35° C. for 12 hours and evaporated under reduced pressure. Water (100 ml) was added to the resulting syrup and the mixture was stirred for 30 minutes. The mixture became thick in the course of stirring. The solid substance was collected by filtration, washed with cold water and recrystallized from aqueous alcohol to give 8.6 g of N-(4-hydroxyphenyl)-N'-methylurea of melting point 169°-171° C.

Quelle