Hydrazine hydrate (1:1) → 6-(4-Fluorophenyl)-3-hydrazinyl-1,2,4-triazine

HRID 2245934Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2245934
O.[NH2:2][NH2:3].Cl[C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=[CH:9][N:10]=1>N1C=CC=CC=1>[F:17][C:14]1[CH:15]=[CH:16][C:11]([C:8]2[N:7]=[N:6][C:5]([NH:2][NH2:3])=[N:10][CH:9]=2)=[CH:12][CH:13]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 213152193-Chloro-6-(4-fluorophenyl)-1,2,4-triazine

Produkt 1

HCID 213152186-(4-Fluorophenyl)-3-hydrazinyl-1,2,4-triazineAusbeute 91,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Hydrazine hydrate (0.28 mL, 0.0057 mol) was added to a suspension of 3-chloro-6-(4-fluorophenyl)-1,2,4-triazine (400 mg, 0.002 mol) in pyridine (4 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 solid was collected and dried under high vacuum to give the desired product (360 mg, 91.9%). Analytical LCMS: (M+H)+=206.1.

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 solid was collected
  8. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f62db4492c314b47a084da69fa75a2ad
Quelldatensatz
uspto-grants-2010_03
Patentnummer
US07683060B2

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