反応 #93228

反応方程式

methyl isocyanate

4-aminophenol

→

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

収率 51.8%

溶媒

acetonitrile

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他evaporated 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
   ろ過The solid substance was collected by filtration
6. 6
   洗浄washed with cold water
7. 7
   その他recrystallized from aqueous alcohol

実験手順

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.

出典