Hydrogen Peroxide → 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfonyl-1H-pyrazole-3-carboxaldehyde oxime

HRID 989223

Reaktionsgleichung

Reaktionsgleichung von HRID 989223
[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([CH:19]=[N:20][OH:21])[C:3]=1[S:22]([CH3:24])=[O:23].[OH:25]O.O>CO.C(O)(=O)C>[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([CH:19]=[N:20][OH:21])[C:3]=1[S:22]([CH3:24])(=[O:25])=[O:23]

Komponenten

5

Edukt 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 1363524165-amino-1-[2,6-dichloro-4-(trifluoromethyl)-phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde oxime

Produkt 1

HCID 1363524175-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfonyl-1H-pyrazole-3-carboxaldehyde oximeAusbeute 64,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 10129899Acetic acid methanolLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

A mixture of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-mehtylsulfinyl-1H-pyrazole-3-carboxaldehyde oxime (1.38 g), 30% hydrogen peroxide (1.38 ml) sodium tungstate dihydrate (0.17 g) in methanol/acetic acid was stirred at 20° C. overnight, then at 50° C. for 4 hours, and again at 20° C. overnight. Water was added and the solid filtered, water-washed and dried to give 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfonyl-1H-pyrazole-3-carboxaldehyde oxime (0.93 g) m.p.209.5-211° C. (decomposition). Compound 16.

Aufarbeitung

  1. waitat 50° C. for 4 hours
  2. customagain at 20° C.
  3. customovernight
  4. filtrationthe solid filtered
  5. washwater-washed
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b43cd4c20c724525bcfd1375a41ad9d0
Quelldatensatz
uspto-grants-2003_10
Patentnummer
US06638956B2

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