HCID 12877066, Verbindung → 74852-82-7

HRID 1154736Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1154736
[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[N:5]=[C:4](SC)[N:3]=1>[Ni].CO>[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[N:5]=[CH:4][N:3]=1

Komponenten

4

Edukt 1

HCID 12877066HCID 12877066, Verbindung

Produkt 1

HCID 1287706874852-82-7Ausbeute 47 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 20 parts of 4-[5-methyl-3-(methylthio)-1H-1,2,4-triazol-1-yl]benzenamine, 15 parts of Raney-nickel catalyst and 400 parts of methanol is stirred and refluxed for 2 hours. The Raney-nickel is filtered off and another 15 parts of the catalyst are added. Stirring at reflux is continued for 4 hours. The reaction mixture is filtered, washed on the filter with methanol and the filtrate is evaporated. The residue is crystallized from a mixture of 4-methyl-2-pentanone, 2,2'-oxybispropane and petroleumether. The product is filtered off and dried, yielding 7.6 parts (47%) of 4-(5-methyl-1H-1,2,4-triazol-1-yl)benzenamine; mp. 145° C.

Aufarbeitung

  1. temperaturerefluxed for 2 hours
  2. filtrationThe Raney-nickel is filtered off
  3. additionanother 15 parts of the catalyst are added
  4. stirringStirring
  5. temperatureat reflux
  6. filtrationThe reaction mixture is filtered
  7. washwashed on the
  8. filtrationfilter with methanol
  9. customthe filtrate is evaporated
  10. customThe residue is crystallized from a mixture of 4-methyl-2-pentanone, 2,2'-oxybispropane and petroleumether
  11. filtrationThe product is filtered off
  12. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a2eee97010ff4746bc3198b73ac267fe
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04490530

Notizen zur Reaktion

Wird geladen…