Potassium Carbonate → HCID 18977189, Verbindung

HRID 1939923Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1939923
C(=O)([O-])[O-].[K+].[K+].Cl.[C:8](Cl)(=[O:15])[C:9]1[CH:14]=[CH:13][CH:12]=[N:11][CH:10]=1.CN(C)C(=O)C.[NH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]1[CH:33]=[CH:32][C:31]([C:34]2[CH2:35][CH2:36][C:37](=[O:40])[NH:38][N:39]=2)=[CH:30][CH:29]=1>O>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([C:8]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]2[CH:29]=[CH:30][C:31]([C:34]3[CH2:35][CH2:36][C:37](=[O:40])[NH:38][N:39]=3)=[CH:32][CH:33]=2)=[O:15])[CH:10]=1

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 18977184HCID 18977184, Verbindung

Produkt 1

HCID 18977189HCID 18977189, VerbindungAusbeute 80,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

At an inner temperature of 0° C., 50 g of anhydrous potassium carbonate and then 8.5 g of nicotinic acid chloride hydrochloride were added to a N,N-dimethylacetamide suspension (270 ml) containing 9.0 g of 6-[4-(4-aminobutyl)phenyl]-4,5-dihydropyridazin-3(2H)-one. The reaction mixture was stirred at the same temperature for 30 minutes and then poured into 200 ml of ice water. After the mixture was stirred at room temperature for 2 hours, water (300 ml) was further added to the mixture, and precipitated crystal was collected by filtration. The resulting crystal was washed with water and then recrystallized from methanol to obtain 10.3 g of 6-[4-(4-(pyridin-3-ylcarbonylamino)butyl)phenyl]-4,5-dihydropyridazin-3(2H)-one.

Aufarbeitung

  1. stirringAfter the mixture was stirred at room temperature for 2 hours
  2. customprecipitated crystal
  3. filtrationwas collected by filtration
  4. washThe resulting crystal was washed with water
  5. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-e67ebe5ecaaa4369938e83315f1a825c
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05698554

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