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3-Acetylpyridine → 1-(3-Pyridinyl)-1-ethanone hydrazone

HRID 1826462
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1826462
[C:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][CH:9]=1)(=O)[CH3:2].O.O.[NH2:12][NH2:13]>O>[N:6]1[CH:7]=[CH:8][CH:9]=[C:4]([C:1](=[N:12][NH2:13])[CH3:2])[CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 95893-AcetylpyridineHCID 22141362Hydrazine--water (1/2)

Produkt 1

HCID 598980421-(3-Pyridinyl)-1-ethanone hydrazoneAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 3-acetylpyridine (6.1 g, 52 mmol) in industrial methylated spirits (50 ml) was added dropwise hydrazine hydrate monohydrate (3.11 ml, 0.1 mol). The reaction mixture was refluxed for 4 h, before cooling to room temperature and stirring for 16 h. Water (25 ml) was added and the volatile organics were removed in vacuo. The predominantly aqueous residual liquor was extracted with ethyl acetate, and the combined organic extracts were dried (Na2SO4) and concentrated to give a yellow oil (5.4 g, 80%) which was taken forward without further purification.

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Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 4 h
  2. customthe volatile organics were removed in vacuo
  3. extractionThe predominantly aqueous residual liquor was extracted with ethyl acetate
  4. dry with materialthe combined organic extracts were dried (Na2SO4)
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-38ecefc1dcb046a093d194d8bb0d3444
Quelldatensatz
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07049444B2

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