4-Amino-1-naphthalenecarbonitrile → 4-Cyano-1-hydrazinonaphthalene

HRID 1441021Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1441021
[N:1]([O-])=O.[Na+].[C:5]([C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([NH2:17])=[CH:9][CH:8]=1)#[N:6]>O.Cl>[C:5]([C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([NH:17][NH2:1])=[CH:9][CH:8]=1)#[N:6]

Komponenten

5

Edukt 2

HCID 428284-Amino-1-naphthalenecarbonitrileHCID 23668193Sodium Nitrite

Produkt 1

HCID 221204294-Cyano-1-hydrazinonaphthalene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel2×HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of 4.09 g of sodium nitrite in 30 ml of water is added to a solution, cooled to 0° C., of 8.35 g of 4-cyano-1-naphthylamine in 180 ml of 1N HCl. The mixture is left stirring for 1 hour 15 minutes at 0° C. It is cooled to -10° C., and a solution of 41.75 g of stannous chloride dihydrate in 42 ml of concentrated HCl is added slowly. The reaction mixture is stirred for 1 hour, allowing the temperature to rise to RT. It is filtered. The residue is suspended in water and 20 ml of concentrated NaOH are added. The expected product is obtained after filtration, rinses with water and then drying under vacuum, m =8.6 g.

Aufarbeitung

  1. waitThe mixture is left
  2. temperatureIt is cooled to -10° C.
  3. stirringThe reaction mixture is stirred for 1 hour
  4. customto rise to RT
  5. filtrationIt is filtered
  6. addition20 ml of concentrated NaOH are added

Quellen und Nachweise

ORD-Eintrag
ord-9504b7d81a1e4d8b93b706a4355a26b6
Quelldatensatz
uspto-grants-1996_03
Patentnummer
US05502059

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