n-Methyl-p-aminophenol → HCID 22401438, 화합물

HRID 260345

반응식

HRID 260345 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 22401438HCID 22401438, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-82e3dd0e1a454b0ea44342105fcbb72d
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527816

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