Hydroxyamine hydrochloride → HCID 86647327, Verbindung

HRID 1880720Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1880720
C(=O)(O)[O-:2].[Na+].Cl.NO.[F:9][C:10]1[N:15]=[C:14]([C:16]#[N:17])[CH:13]=[C:12]([C:18]([F:21])([F:20])[F:19])[CH:11]=1>C(O)C>[F:9][C:10]1[N:15]=[C:14]([C:16]([NH2:17])=[O:2])[CH:13]=[C:12]([C:18]([F:21])([F:19])[F:20])[CH:11]=1

Komponenten

5

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 534388006-Fluoro-4-(trifluoromethyl)pyridine-2-carbonitrile

Produkt 1

HCID 86647327HCID 86647327, VerbindungAusbeute 78,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To 9 ml of ethanol were added 0.73 g of sodium bicarbonate and 0.61 g of hydroxylamine hydrochloride, and the mixture was heated to reflux for 1 hour. After allowing to cool, 0.7 g of 6-fluoro-4-trifluoromethylpyridine-2-carbonitrile was added at 0° C., and the mixture was stirred, 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 6-fluoro-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-3feb899d51be438883734f093f668ebd
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08318776B2

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