Hydrazine hydrate (1:1) → 2,4,5-Trifluoro-3-methoxyaniline

HRID 358871Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 358871
O.NN.[CH3:4][O:5][C:6]1[C:7]([F:25])=[C:8]([N:14]2C(=O)C3=CC=CC=C3C2=O)[CH:9]=[C:10]([F:13])[C:11]=1[F:12]>C(O)C>[CH3:4][O:5][C:6]1[C:7]([F:25])=[C:8]([CH:9]=[C:10]([F:13])[C:11]=1[F:12])[NH2:14]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 20067133N-(3-Methoxy-2,4,5-trifluorophenyl)-phthalimide

Produkt 1

HCID 27752772,4,5-Trifluoro-3-methoxyanilineAusbeute 85,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1.1 g (0.02 mole) of hydrazine hydrate was added to a suspension of 2.15 g (0.007 mole) of N-(3-methoxy-2,4,5-trifluorophenyl)phthalimide (XXXVI) [prepared as described in Step (F3) above] in 30 ml of ethanol, and the mixture was heated under reflux with stirring for 2 hours. The reaction mixture was cooled to room temperature and then filtered. The filtrate was concentrated by evaporation under reduced pressure, and the residue was dissolved in toluene. The resulting solution was washed with water and dried, and the solvent was then removed by evaporation under reduced pressure to afford 1.06 g of 3-methoxy-2,4,5-trifluoroaniline (XXIII) as pale brown needles.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated by evaporation under reduced pressure
  5. dissolutionthe residue was dissolved in toluene
  6. washThe resulting solution was washed with water
  7. customdried
  8. customthe solvent was then removed by evaporation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4e78f93e281f4646b98739d707826e81
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US04997943

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