Hydrazine hydrate (1:1) → 3-Hydrazino-6-phenyl-1,2,4-triazine

HRID 607550Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 607550
O.[NH2:2][NH2:3].Cl[C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][N:10]=1>N1C=CC=CC=1>[NH:2]([C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][N:10]=1)[NH2:3]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 110306323-Chloro-6-phenyl-1,2,4-triazine

Produkt 1

HCID 64051603-Hydrazino-6-phenyl-1,2,4-triazineAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Hydrazine hydrate (1.50 mL, 0.0308 mol) was added to suspension of 3-chloro-6-phenyl-1,2,4-triazine (2.20 g, 0.0115 mol) in pyridine (12.0 mL) at 0° C. and stirred at 0° C. until a precipitate formed. The mixture was then heated at 65° C. for 30 min. The solvent was evaporated under reduced pressure. The residue was triturated with water, filtered, and washed with water. The crystalline formed was collected and dried under high vacuum to give the desired product (2.0 g, 93%). Analytical LCMS: (M+H)+=188.1.

Aufarbeitung

  1. customformed
  2. temperatureThe mixture was then heated at 65° C. for 30 min
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue was triturated with water
  5. filtrationfiltered
  6. washwashed with water
  7. customThe crystalline formed
  8. customwas collected
  9. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-25b497d407434321bda51f0a6d3e8ca1
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07915408B2

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