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Water → HCID 22934879, Verbindung

HRID 254206
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 254206
[CH3:1][S:2][O-].[Na+].[Cl:5][CH2:6][C:7]1([CH3:26])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([C:22]([F:25])([F:24])[F:23])=[N:16][N:17]([CH2:20][CH3:21])[C:18]=2F)[CH2:8]1.O.C(OCC)(=O)C>CN(C)C=O>[Cl:5][CH2:6][C:7]1([CH3:26])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([C:22]([F:25])([F:24])[F:23])=[N:16][N:17]([CH2:20][CH3:21])[C:18]=2[S:2][CH3:1])[CH2:8]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 22934872HCID 22934872, VerbindungHCID 23717576HCID 23717576, Verbindung

Produkt 1

HCID 22934879HCID 22934879, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228Dimethylformamide
Lösungsmittel

Versuchsvorschrift

4.21 g (9.0 mmoles) of sodium methyl thioalcoholate (in the form of a 15% aqueous solution) was added, at room temperature, into a solution of 1.08 g (3.0 mmoles) of 5-chloromethyl-3-(1-ethyl-5-fluoro-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5-methyl-2-isoxazoline dissolved in 10 ml of N,N-dimethylformamide. The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into water and extraction with ethyl acetate was conducted. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein to obtain a crude product of 5-chloromethyl-3-(1-ethyl-5-methylthio-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5-methyl-2-isoxazoline.

Aufarbeitung

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. washThe resulting organic layer was washed with water
  5. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to reduced pressure distillation
  7. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-af80fb8dc5f74387a818711b6532b502
Quelldatensatz
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07875606B2

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