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Pyridine-2-carbonitrile → Cqp4A25CE2

HRID 1171168
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1171168
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)#[N:2].O.[NH2:10][NH2:11]>CCO>[CH:7]1[CH:8]=[C:3](/[C:1](/[NH2:2])=[N:10]\[NH2:11])[N:4]=[CH:5][CH:6]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 7522Pyridine-2-carbonitrileHCID 24654Hydrazine hydrate (1:1)

Produkt 1

HCID 5481389Cqp4A25CE2Ausbeute 137,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

2-Cyano pyridine (500 mg, 1.923 mmol) and Hydrazine hydrate (252 mg, 1.923 mmol) were mixed together in EtOH (3 ml). The clear solution was left at 15° C. (in refrigerator) for 18 h (Monitored by TLC). Ethanol was concentrated under reduced pressure and then the reaction mixture was diluted with diethyl ether (50 ml) and water. The diethyl ether layer was separated, washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to 1/5th Volume. The ethereal solution was cooled to 0° C. and the obtained solid precipitate was collected over the filtration and dried under vacuum, which gave the 2-pyridine Amidrazone (360 mg).

Aufarbeitung

  1. concentrationEthanol was concentrated under reduced pressure
  2. additionthe reaction mixture was diluted with diethyl ether (50 ml) and water
  3. customThe diethyl ether layer was separated
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure to 1/5th Volume
  8. filtrationthe obtained solid precipitate was collected over the filtration
  9. customdried under vacuum, which

Quellen und Nachweise

ORD-Eintrag
ord-69fecea4563a43a794e7340f3caa5c4e
Quelldatensatz
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07829589B2

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