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

HRID 1589136ノート

反応式

HRID 1589136 の反応式
[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

参加物

5

反応物 2

HCID 4034-AminophenolHCID 12228Methyl Isocyanate

生成物 1

HCID 3496051-(4-hydroxyphenyl)-3-methylurea収率 51.8%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6342Acetonitrile溶媒

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.

後処理

  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

出典と根拠

ORDレコード
ord-ef58c3d163654dcf95f4fa04007ec3d2
出典データセット
uspto-grants-1986_02
特許番号
US04568674

反応ノート

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