Methanol → R 61837

HRID 486471Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 486471
[CH3:1][O-:2].[Na+].[Na].CO.Cl[C:8]1[N:9]=[N:10][C:11]([N:14]2[CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[CH:21]=3)[CH2:16][CH2:15]2)=[CH:12][CH:13]=1>O>[CH3:1][O:2][C:8]1[N:9]=[N:10][C:11]([N:14]2[CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[CH:21]=3)[CH2:16][CH2:15]2)=[CH:12][CH:13]=1

Komponenten

6

Edukt 4

HCID 887MethanolHCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 15124568HCID 15124568, Verbindung

Produkt 1

HCID 127504R 61837Ausbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred sodium methoxide solution, previously prepared starting from 1.6 parts of sodium in 24 parts of methanol, were added 4 parts of 3-chloro-6-[4-(3-methylphenyl)-1-piperazinyl]pyridazine. The whole was stirred and refluxed for 40 hours. After cooling 25 parts of water were added. The product was filtered off, washed with water and dissolved in trichloromethane. The organic layer was dried, filtered and evaporated. The residue was crystallized from a mixture of 2-propanol and 2,2'-oxybispropane. The product was filtered off and dried, yielding 2 parts (50%) of 3-methoxy-6-[4-(3-methylphenyl)-1-piperazinyl]pyridazine; mp. 137.1° C. (compound 258).

Aufarbeitung

  1. temperaturerefluxed for 40 hours
  2. additionwere added
  3. filtrationThe product was filtered off
  4. washwashed with water
  5. dissolutiondissolved in trichloromethane
  6. customThe organic layer was dried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was crystallized from a mixture of 2-propanol and 2,2'-oxybispropane
  10. filtrationThe product was filtered off
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b37c733004fb47d69e99b4a7c5fadde4
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05292738

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