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Water → HCID 86612666, Verbindung

HRID 1982980
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1982980
Cl[CH2:2][N:3]1[CH:7]=[N:6][C:5]([C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])=[N:4]1.[CH2:15]([CH:18]([C:21]#[N:22])[C:19]#[N:20])[CH:16]=[CH2:17].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:15]([C:18]([CH2:2][N:3]1[CH:7]=[N:6][C:5]([C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])=[N:4]1)([C:21]#[N:22])[C:19]#[N:20])[CH:16]=[CH2:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 10931386HCID 10931386, VerbindungHCID 23149134HCID 23149134, Verbindung

Produkt 1

HCID 86612666HCID 86612666, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228Dimethylformamide
Lösungsmittel

Versuchsvorschrift

1-(chloromethyl)-3-(pentafluoroethyl)-1H-1,2,4-triazole and 1.02 g of allyl malononitrile were dissolved in 28 ml of N,N-dimethylformamide. 2.76 g of potassium carbonate was added to the solution under ice cooling with stirring, followed by stirring at room temperature for overnight. Water was added to the reaction mixture, and then extracted with MTBE. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and then subjected to preparative high performance liquid chromatography to obtain 0.54 g of allyl {[3-(pentafluoroethyl)-1H-1,2,4-triazole 1-yl]methyl}malononitrile (referred as the compound of the present invention (35), hereinafter) shown by below formula.

Aufarbeitung

  1. stirringby stirring at room temperature for overnight
  2. extractionextracted with MTBE
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e641bc190ef24d2a93f61bb2617f2eb8
Quelldatensatz
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07541374B2

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