n-Methyl-p-aminophenol → HCID 22401438、化合物

HRID 260345

反応式

HRID 260345 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[C:10](OC(=O)C)(=[O:12])[CH3:11].[C:17]([O-])(=[O:19])[CH3:18].[Na+].C(=O)(O)[O-].[Na+]>O.C(O)(=O)C>[C:10]([O:9][C:6]1[CH:7]=[CH:8][C:3]([N:2]([C:17](=[O:19])[CH3:18])[CH3:1])=[CH:4][CH:5]=1)(=[O:12])[CH3:11]

参加物

7

反応物 4

HCID 5931n-Methyl-p-aminophenolHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 517045Sodium Acetate

生成物 1

HCID 22401438HCID 22401438、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

To a flask was added 20.0 g. of 4-(N-methylamino)phenol, 20 ml. of acetic anhydride, 60 ml. of acetic acid and 10 g. of sodium acetate. The solution was warmed on a steam bath for one hour and water added to clarify the solution. The mixture was allowed to cool, more water added and the resulting solution poured onto solid sodium bicarbonate in an open vessel. The aqueous material was extracted five times with 200 ml. portions of ethyl ether, the ether extracts combined, washed with brine, then dried and concentrated to obtain the crude 4-(N-acetyl-N-methylamino)phenyl acetate which was recrystallized from a mixture of ethyl acetate, hexane and ethanol.

後処理

  1. additionTo a flask was added 20.0 g
  2. temperatureThe solution was warmed on a steam bath for one hour
  3. temperatureto cool
  4. extractionThe aqueous material was extracted five times with 200 ml
  5. washwashed with brine
  6. customdried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-82e3dd0e1a454b0ea44342105fcbb72d
出典データセット
uspto-grants-1996_06
特許番号
US05527816

関連ノート

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