Ammonium Hydroxide → Flupoxam

HRID 1647919

Reaktionsgleichung

Reaktionsgleichung von HRID 1647919
[NH4+:1].[OH-].[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][N:11]=[C:12]2[C:16](=O)[O:15][C:14]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:13]2)=[CH:6][C:5]=1[CH2:24][O:25][CH2:26][C:27]([F:33])([F:32])[C:28]([F:31])([F:30])[F:29]>O>[Cl:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[C:14]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:13][C:12]([C:16]([NH2:1])=[O:15])=[N:11]2)=[CH:6][C:5]=1[CH2:24][O:25][CH2:26][C:27]([F:32])([F:33])[C:28]([F:31])([F:30])[F:29]

Komponenten

4

Edukt 2

HCID 14923Ammonium HydroxideHCID 1785190634-[[4-chloro-3-(2,2,3,3,3-pentafluoropropoxymethyl)phenyl]hydrazinylidene]-2-phenyl-1,3-oxazol-5-one

Produkt 1

HCID 86353FlupoxamAusbeute 100,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A 29% ammonia aqueous solution (3.48 kg, 59.2 mol) was added to 47.8 kg of water. 2-phenyl-4,5-oxazoledione 4-[4-chloro-3-(2,2,3,3,3-pentafluoropropoxy)methylphenyl]hydrazone (14.9 kg, purity: 94.4%, water content: 36.5%, 19.4 mol) was added to the solution and the mixture was heated while stirring. After heating at 80° C. for two hours (after three hours after initiation of the heating), the reaction mixture was cooled to 50° C. and filtered by centrifugation. The residue was washed with hot water dried in a hot air drier to obtain 9.0 kg of the target compound.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperaturewas cooled to 50° C.
  3. filtrationfiltered by centrifugation
  4. washThe residue was washed with hot water
  5. customdried in a hot air drier

Quellen und Nachweise

ORD-Eintrag
ord-d35567e597564bb68a991e70b4b1f450
Quelldatensatz
uspto-grants-1995_07
Patentnummer
US05434268

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