Hydrazine → 2-Hydrazinyl-5-nitropyridine

HRID 261271

Reaktionsgleichung

Reaktionsgleichung von HRID 261271
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[NH2:11][NH2:12]>CO.O>[NH:11]([C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1)[NH2:12]

Komponenten

5

Edukt 2

HCID 9321HydrazineHCID 783082-Chloro-5-nitropyridine

Produkt 1

HCID 40319312-Hydrazinyl-5-nitropyridine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

To a slurry of 47.6 g (0.3 mol) of 2-chloro-5-nitropyridine in a mixture of 400 ml methanol and 60 ml water and cooled to 10° C. was added with cooling below 30° 86 g hydrazine (95 percent) over about 10 minutes. The solids first went into solution, then a greenish-yellow precipitate separated. The mixture was stirred at reflux for 30 minutes. The greenish solid was filtered off and washed with cold methanol. The solid was slurried in 200 ml of cold water, washed and vacuum dried. The yield was 40.1 g (87 percent).

Aufarbeitung

  1. additionwas added
  2. customa greenish-yellow precipitate separated
  3. temperatureat reflux for 30 minutes
  4. filtrationThe greenish solid was filtered off
  5. washwashed with cold methanol
  6. washwashed
  7. customvacuum dried

Quellen und Nachweise

ORD-Eintrag
ord-8b02e0cb6f5744d5ad1be18e9dfdc670
Quelldatensatz
uspto-grants-1979_08
Patentnummer
US04165238

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