Triethylamine → 3-[4-(3-Methylphenyl)-1-piperazinyl]-6-(methylsulfonyl)pyridazine

HRID 466562

Reaktionsgleichung

Reaktionsgleichung von HRID 466562
Cl[C:2]1[N:3]=[N:4][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[CH:6][CH:7]=1.[CH3:12][C:13]1[CH:14]=[C:15]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)[CH:16]=[CH:17][CH:18]=1.C(N(CC)CC)C>C1C=CC=CC=1>[CH3:12][C:13]1[CH:14]=[C:15]([N:19]2[CH2:24][CH2:23][N:22]([C:2]3[N:3]=[N:4][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[CH:6][CH:7]=3)[CH2:21][CH2:20]2)[CH:16]=[CH:17][CH:18]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 831111-(m-Tolyl)piperazineHCID 2524763-Chloro-6-(methylsulfonyl)pyridazine

Produkt 1

HCID 151246013-[4-(3-Methylphenyl)-1-piperazinyl]-6-(methylsulfonyl)pyridazineAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A mixture of 3.2 parts of 3-chloro-6-(methylsulfonyl)pyridazine, 3 parts of 1-(3-methylphenyl)piperazine, 2 parts of N,N-diethylethanamine and 180 parts of benzene was stirred for 24 hours at reflux. The reaction mixture was evaporated. Water was added to the residue. The precipitated product was filtered off, washed with water and dissolved in trichloromethane. The solution was dried, filtered and evaporated. The residue was crystallized from methanol. The product was filtered off and dried, yielding 5 parts (89%) of 3-[4-(3-methylphenyl)-1-piperazinyl]-6-(methylsulfonyl)pyridazine; mp. 201° C. (compound 209).

Aufarbeitung

  1. temperatureat reflux
  2. customThe reaction mixture was evaporated
  3. additionWater was added to the residue
  4. filtrationThe precipitated product was filtered off
  5. washwashed with water
  6. dissolutiondissolved in trichloromethane
  7. customThe solution was dried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue was crystallized from methanol
  11. filtrationThe product was filtered off
  12. customdried

Quellen und Nachweise

ORD-Eintrag
ord-4747d6ab4c074086be6054a49c67d4fd
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05157035

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