5,5-dimethyl-3-(3-methoxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline → 5,5-dimethyl-3-(3-hydroxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline

HRID 1172070Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1172070
C(O)(=O)C.Br.[CH3:6][C:7]1([CH3:26])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([O:24]C)=[N:16][N:17]([CH3:23])[C:18]=2[C:19]([F:22])([F:21])[F:20])[CH2:8]1>>[CH3:6][C:7]1([CH3:26])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([OH:24])=[N:16][N:17]([CH3:23])[C:18]=2[C:19]([F:22])([F:21])[F:20])[CH2:8]1

Komponenten

3

Edukt 2

HCID 178628515,5-dimethyl-3-(3-methoxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazolineHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

Produkt 1

HCID 1784819505,5-dimethyl-3-(3-hydroxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazolineAusbeute 96 %

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To 20 ml of a 25% hydrogen bromide acetic acid solution was added 3.3 g (10.6 mmoles) of 5,5-dimethyl-3-(3-methoxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline. The mixture was stirred at 50° C. for 3 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was subjected to vacuum distillation to remove the solvent contained therein. The residue was poured into water. The resulting crystals were collected by filtration, washed with water and dried to obtain 3.1 g (yield: 96.0%) of intended 5,5-dimethyl-3-(3-hydroxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline.

Aufarbeitung

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. distillationthe reaction mixture was subjected to vacuum distillation
  5. customto remove the solvent
  6. additionThe residue was poured into water
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with water
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-699948a3dbe240c4afddbc07931d26f5
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07833939B2

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