Water → 3,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone)

HRID 48483

Reaktionsgleichung

Reaktionsgleichung von HRID 48483
C([O-])(=O)C.[Na+].O.Br[CH:8](Br)[C:9]([C:11]([F:14])([F:13])[F:12])=[O:10].[F:16][C:17]1[CH:22]=[C:21]([Cl:23])[C:20]([O:24][CH:25]([CH3:27])[CH3:26])=[CH:19][C:18]=1[NH:28][NH2:29]>C(OCC)C>[Cl:23][C:21]1[C:20]([O:24][CH:25]([CH3:26])[CH3:27])=[CH:19][C:18]([NH:28][N:29]=[CH:8][C:9](=[O:10])[C:11]([F:14])([F:13])[F:12])=[C:17]([F:16])[CH:22]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 185080(4-Chloro-2-fluoro-5-propan-2-yloxyphenyl)hydrazineHCID 517045Sodium AcetateHCID 5505231,1-Dibromo-3,3,3-trifluoroacetone

Produkt 1

HCID 691414303,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To a mixed solution of 5.3 g (53.5 mmol) of sodium acetate and about 100 ml of water was added under ice cooling 6.6 g (24.3 mmol) of 1,1-dibromo-3,3,3-trifluoroacetone, and the reaction was allowed to proceed at 70° C. for 20 minutes. Then, the reaction mixture was cooled to room temperature, to which a solution of 5.8 g (21.5 mmol) of 2-fluoro-4-chloro-5-isopropoxyphenylhydrazine dissolved in about 20 ml of diethyl ether was added, and the reaction mixture was stirred at room temperature for 1 hour. The ether layer was separated, washed once with 10 ml of saturated sodium chloride solution, and dried with magnesium sulfate. The diethyl ether was distilled out, which afforded 6.5 g (20.0 mmol) of 3,3,3-trifluoro-2-oxo-propanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone).

Aufarbeitung

  1. additionwas added
  2. customThe ether layer was separated
  3. washwashed once with 10 ml of saturated sodium chloride solution
  4. dry with materialdried with magnesium sulfate
  5. distillationThe diethyl ether was distilled out

Quellen und Nachweise

ORD-Eintrag
ord-285974394a6940eb86913218fa000983
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06703503B2

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