m-Chloroperbenzoic acid → HCID 86644470, Verbindung

HRID 2404539Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2404539
[Cl:1][C:2]1[C:3]([O:23][C:24]([F:32])([F:31])[CH:25]([F:30])[C:26]([F:29])([F:28])[F:27])=[N:4][N:5]([C:9]2[CH:14]=[C:13]([S:15][CH2:16][C:17]([F:20])([F:19])[F:18])[C:12]([CH3:21])=[CH:11][C:10]=2[F:22])[C:6]=1[NH:7][CH3:8].ClC1C=CC=C(C(OO)=[O:41])C=1>C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([O:23][C:24]([F:31])([F:32])[CH:25]([F:30])[C:26]([F:27])([F:28])[F:29])=[N:4][N:5]([C:9]2[CH:14]=[C:13]([S:15]([CH2:16][C:17]([F:20])([F:19])[F:18])=[O:41])[C:12]([CH3:21])=[CH:11][C:10]=2[F:22])[C:6]=1[NH:7][CH3:8]

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 86644469HCID 86644469, Verbindung

Produkt 1

HCID 86644470HCID 86644470, VerbindungAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

0.24 g of 4-chloro-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-(1,1,2,3,3,3-hexafluoropropoxy)-5-methylaminopyrazole was dissolved in 10 mL of chloroform, and 120 mg of m-chloroperbenzoic acid (purity: 75%) was added under cooling with ice. After stirring for one hour under cooling with ice, the solution was washed with an aqueous sodium thiosulfate solution and then washed with an aqueous sodium hydrogen carbonate solution, and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:2) to obtain 0.24 g of 4-chloro-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylsulfinyl)phenyl}-3-(1,1,2,3,3,3-hexafluoropropoxy)-5-methylaminopyrazole.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. washthe solution was washed with an aqueous sodium thiosulfate solution
  4. washwashed with an aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThen, the solvent was distilled off under reduced pressure
  7. customthe obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:2)

Quellen und Nachweise

ORD-Eintrag
ord-cecdae981d094af3ba1519500504cfcf
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08802713B2

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