Benzaldehyde → HCID 54443969, Verbindung

HRID 261074

Reaktionsgleichung

Reaktionsgleichung von HRID 261074
[CH3:1][NH:2][NH2:3].[CH:4](=O)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH3:12][S:13][C:14](=[C:17]([C:20]#[N:21])[C:18]#[N:19])SC>COCCO>[CH3:1][N:2]([C:14]([S:13][CH3:12])=[C:17]([C:20]#[N:21])[C:18]#[N:19])[N:3]=[CH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

5

Edukt 3

HCID 240BenzaldehydeHCID 6061MethylhydrazineHCID 992292-(Bis(methylsulfanyl)methylidene)propanedinitrile

Produkt 1

HCID 54443969HCID 54443969, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80192-MethoxyethanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Methyl hydrazine (4.2 g) was added slowly to benzaldehyde (9.4 ml) in 2-methoxyethanol (15 ml) causing the solution to boil. The solution was heated under reflux for 20 minutes and was then added to a solution of bis(methylmercapto)methylenemalononitrile (15.6 g) in 2-methoxyethanol (75 ml). The solution was heated under reflux for 6 hours and was then cooled to 0° C. to precipitate benzaldehyde N-methyl-N-(2,2-dicyano-1-methylmercaptoethenyl) hydrazone (5.6 g), m.p. 159°-160° C.

Aufarbeitung

  1. temperatureThe solution was heated
  2. temperatureunder reflux for 20 minutes
  3. temperatureThe solution was heated
  4. temperatureunder reflux for 6 hours
  5. customto precipitate benzaldehyde N-methyl-N-(2,2-dicyano-1-methylmercaptoethenyl) hydrazone (5.6 g), m.p. 159°-160° C.

Quellen und Nachweise

ORD-Eintrag
ord-af57ceba72d4402a894e010ee4dbe617
Quelldatensatz
uspto-grants-1979_08
Patentnummer
US04163846

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