Ammonia → HCID 70509051, Verbindung

HRID 46558

Reaktionsgleichung

Reaktionsgleichung von HRID 46558
N.[Na].[C:3](#[N:5])[CH3:4].[Cl:6][C:7]1[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=1[C:9]#[N:10]>O1CCCC1.CCOCC>[NH2:10][C:9]([C:8]1[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=1[Cl:6])=[CH:4][C:3]#[N:5]

Komponenten

7

Edukt 4

HCID 222Ammonia2×HCID 6342AcetonitrileHCID 133912-ChlorobenzonitrileHCID 5360545Sodium2×

Produkt 1

HCID 70509051HCID 70509051, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A 150 ml. portion of ammonia is condensed in a reaction flash and a small piece of sodium is added. The blue color is discharged by the addition of ferric chloride and 3.22 g. of sodium are added. After the cooler is discharged 5.75 ml. of acetonitrile in 10 ml. of ether are added. The reaction is cooled in a dry ice-acetone bath and 13.3 g. of 2-chlorobenzonitrile in 25 ml. of tetrahydrofuran are added dropwise. The ammonia is allowed to evaporate, the solvent is blown off with nitrogen and water is added. The mixture is extracted with methylene chloride. The organic extracts are dried over sodium sulfate and filtrate through magnesol. The filtrate is evaporated with the addition of hexanes giving β-amino-2-chlorocinnamonitrile as a white crystalline solid.

Aufarbeitung

  1. customcondensed
  2. customin a reaction flash
  3. temperatureThe reaction is cooled in a dry ice-acetone bath
  4. customto evaporate
  5. additionis added
  6. extractionThe mixture is extracted with methylene chloride
  7. dry with materialThe organic extracts are dried over sodium sulfate and filtrate through magnesol
  8. customThe filtrate is evaporated with the addition of hexanes

Quellen und Nachweise

ORD-Eintrag
ord-23f0bc903b604442a2836b50948d5be0
Quelldatensatz
uspto-grants-1979_11
Patentnummer
US04173650

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