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Hydroxyamine hydrochloride → HCID 86647328, Verbindung

HRID 1880724
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1880724
C(=O)(O)[O-:2].[Na+].Cl.NO.[Cl:9][C:10]1[C:11]([C:18]([F:21])([F:20])[F:19])=[CH:12][C:13]([C:16]#[N:17])=[N:14][CH:15]=1>C(O)C>[Cl:9][C:10]1[C:11]([C:18]([F:21])([F:19])[F:20])=[CH:12][C:13]([C:16]([NH2:17])=[O:2])=[N:14][CH:15]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 595703895-Chloro-4-(trifluoromethyl)-2-pyridinecarbonitrile

Produkt 1

HCID 86647328HCID 86647328, VerbindungAusbeute 74,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To 7 ml of ethanol were added 0.61 g of sodium bicarbonate and 0.5 g of hydroxylamine hydrochloride, and the mixture was heated to reflux for 1 hour. After allowing to cool, 0.74 g of 5-chloro-4-trifluoromethylpyridine-2-carbonitrile was added at 0° C., and the mixture was stirred for 5 hours, and concentrated. To the residue was added water, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.6 g of 5-chloro-4-trifluoromethylpyridine-2-carboxamide=oxime.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 1 hour
  3. temperatureto cool
  4. concentrationconcentrated
  5. additionTo the residue was added water
  6. extractionthe resultant solution was extracted with ethyl acetate three times
  7. washwashed with an aqueous saturated sodium chloride solution
  8. dry with materialdried with anhydrous magnesium sulfate
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-39340d6a9dc44218b70391b56a6108c7
Quelldatensatz
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08318776B2

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