4-Aminophenol → HCID 19792673, Verbindung

HRID 1655550

Reaktionsgleichung

Reaktionsgleichung von HRID 1655550
[F:1][CH:2]=[C:3]([F:5])[F:4].[CH:6]1[C:11]([NH2:12])=[CH:10][CH:9]=[C:8]([OH:13])[CH:7]=1.[OH-].[K+]>CN(C=O)C>[F:4][C:3]([F:5])([O:13][C:8]1[CH:9]=[CH:10][C:11]([NH2:12])=[CH:6][CH:7]=1)[CH2:2][F:1]

Komponenten

5

Edukt 3

HCID 4034-AminophenolHCID 9665TrifluoroethyleneHCID 14797Potassium Hydroxide

Produkt 1

HCID 19792673HCID 19792673, VerbindungAusbeute 25 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Gaseous trifluoroethylene was bubbled into a mixture of 7.0 g (64.1 mmol) of p-aminophenol, 0.7 g (12.8 mmol) of powdered KOH, and 70 ml dry DMF at 90° C. for 11/4 hours. The mixture was poured into ice water and extracted 2 times with ether. The combined ether layers were washed with diluted aqueous NaOH, washed with water, dried over MgSO4 and filtered. HCl was bubbled into the ether solution. The resulting gray solid was collected by filtration to give 3.6 g (25 percent of theoretical) of the above-named aniline as the HCl salt along with a 20 percent impurity of 4-(1,2-difluoroethenyloxy)benzene-amine.

Aufarbeitung

  1. extractionextracted 2 times with ether
  2. washThe combined ether layers were washed with diluted aqueous NaOH
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customHCl was bubbled into the ether solution
  7. filtrationThe resulting gray solid was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-b6d402b15d8b4fe29491860fc02ae96b
Quelldatensatz
uspto-grants-1993_10
Patentnummer
US05250690

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