Dimethylcarbamoyl Chloride → 1-Dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole

HRID 263125Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 263125
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]1[N:11]=[C:10]([C:12]2[CH:17]=[N:16][CH:15]=[CH:14][N:13]=2)[NH:9][N:8]=1.[H-].[Na+].[CH3:20][N:21]([CH3:25])[C:22](Cl)=[O:23]>O1CCCC1>[CH3:20][N:21]([CH3:25])[C:22]([N:8]1[C:7]([C:2]2[CH:3]=[N:4][CH:5]=[CH:6][N:1]=2)=[N:11][C:10]([C:12]2[CH:17]=[N:16][CH:15]=[CH:14][N:13]=2)=[N:9]1)=[O:23]

Komponenten

5

Edukt 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 24758Sodium hydrideHCID 135247872-(5-pyrazin-2-yl-4H-1,2,4-triazol-3-yl)pyrazine

Produkt 1

HCID 202857801-Dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To 2.25 g. (0.01 mole) of 3,5-dipyrazinyl-1,2,4-triazole in 200 ml. of tetrahydrofuran is added 57% sodium hydride (0.42 g., 0.01 mole). The reaction mixture is heated at reflux for one hour, cooled, and a solution of dimethylcarbamoyl chloride (1 gram, 0.01 mole) in 10 ml. of tetrahydrofuran is added dropwise. The reaction mixture is then refluxed four hours, cooled, filtered and concentrated to a solid. After recrystallization from benzene 1-dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole is obtained.

Aufarbeitung

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for one hour
  3. temperaturecooled
  4. temperatureThe reaction mixture is then refluxed four hours
  5. temperaturecooled
  6. filtrationfiltered
  7. concentrationconcentrated to a solid
  8. customAfter recrystallization from benzene 1-dimethylcarbamoyl-3,5-dipyrazinyl-1,2,4-triazole
  9. customis obtained

Quellen und Nachweise

ORD-Eintrag
ord-586d2729ec4446138fe3f9a9f0e441c0
Quelldatensatz
uspto-grants-1979_05
Patentnummer
US04156085

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