Ethanol → [(E)-3-[4-chloro-3-(trifluoromethyl)phenyl]prop-2-enoyl]-oxidoazanium

HRID 1081387Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1081387
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([CH:6]=[CH:7]C#N)=[CH:4][C:3]=1[C:12]([F:15])([F:14])[F:13].Cl.[NH2:17][OH:18].[C:19](=[O:22])([O-])[O-].[Na+].[Na+].C(O)C>O>[Cl:1][C:2]1[CH:11]=[CH:10][C:5](/[CH:6]=[CH:7]/[C:19]([NH2:17]=[O:18])=[O:22])=[CH:4][C:3]=1[C:12]([F:15])([F:14])[F:13]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 541762263-[4-Chloro-3-(trifluoromethyl)phenyl]prop-2-enenitrile

Produkt 1

HCID 23364570[(E)-3-[4-chloro-3-(trifluoromethyl)phenyl]prop-2-enoyl]-oxidoazaniumAusbeute 39,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

12.1 g (0.05 mol) of 4-chloro-3-trifluoromethyl-cinnamonitrile are added to a solution of 7.2 g (0.10 mol) of hydroxylamine hydrochloride, 7.3 g (0.10 mol) of sodium carbonate in 100 ml of water, and 100 ml of ethanol. The mixture is refluxed until the reaction is complete (24 hours) and the entire batch is subsequently stirred into 250. ml of water. The solid which separates out during this process is filtered off with suction, washed with a little water and dried. 5.3 g (39.3 % of theory) of (E)-4-chloro-3-trifluoromethyl-cinnamamide oxide are obtained.

Aufarbeitung

  1. temperatureThe mixture is refluxed until the reaction
  2. custom(24 hours)
  3. filtrationis filtered off with suction
  4. washwashed with a little water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-fbc2a323404447228743f7da6d7b363f
Quelldatensatz
uspto-grants-1996_12
Patentnummer
US05585493

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