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Sodium Hydroxide → HCID 178517757, Verbindung

HRID 1668842
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1668842
[OH-:1].[Na+].[Cl:3][C:4]1[CH:5]=[C:6]([F:11])[C:7](F)=[N:8][CH:9]=1>O>[Cl:3][C:4]1[CH:5]=[C:6]([F:11])[C:7]([OH:1])=[N:8][CH:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 27832485-Chloro-2,3-difluoropyridine

Produkt 1

HCID 178517757HCID 178517757, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of NaOH (101 g, 2.5 mol) in water (500 mL) was added 5-chloro-2,3-difluoropyridine (101 g, 0.68 mol) as a liquid, and the resulting mixture was heated to reflux overnight. After cooling to room temperature, the mixture was filtered through a pad of celite and the pH was adjusted to 1 by the addition of concentrated HCl. The resulting solid was dissolved in ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. The title compound was obtained as a white solid (78 g, 78%) and was used without additional purification. The product was characterized by 1H NMR.

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Aufarbeitung

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux overnight
  3. filtrationthe mixture was filtered through a pad of celite
  4. additionthe pH was adjusted to 1 by the addition of concentrated HCl
  5. dissolutionThe resulting solid was dissolved in ethyl acetate
  6. dry with materialThe combined organic layers were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d1b23ca985b24f128fcbf4a55964425e
Quelldatensatz
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07989469B2

Notizen zur Reaktion

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