4-Aminophenol → 1-(4-hydroxyphenyl)-3-methylurea

HRID 1589136노트

반응식

HRID 1589136 반응식
[CH3:1][N:2]=[C:3]=[O:4].[NH2:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1>C(#N)C.CN(C)C=O>[OH:12][C:9]1[CH:10]=[CH:11][C:6]([NH:5][C:3]([NH:2][CH3:1])=[O:4])=[CH:7][CH:8]=1

참가 물질

5

반응물 2

HCID 4034-AminophenolHCID 12228Methyl Isocyanate

생성물 1

HCID 3496051-(4-hydroxyphenyl)-3-methylurea수율 51.8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  1. customevaporated under reduced pressure
  2. additionWater (100 ml) was added to the resulting syrup
  3. stirringthe mixture was stirred for 30 minutes
  4. stirringof stirring
  5. filtrationThe solid substance was collected by filtration
  6. washwashed with cold water
  7. customrecrystallized from aqueous alcohol

출처 및 근거

ORD 기록
ord-ef58c3d163654dcf95f4fa04007ec3d2
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04568674

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