Water → 1,2-Dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-pyridine

HRID 414315

Reaktionsgleichung

Reaktionsgleichung von HRID 414315
[CH3:1][C:2]1[NH:7][C:6](=[O:8])[C:5](C#N)=[CH:4][C:3]=1[C:11]1[CH:12]=[CH:13][C:14]2[N:15]([CH:17]=[CH:18][N:19]=2)[CH:16]=1.O.O.N>P(=O)(O)(O)O>[CH3:1][C:2]1[NH:7][C:6](=[O:8])[CH:5]=[CH:4][C:3]=1[C:11]1[CH:12]=[CH:13][C:14]2[N:15]([CH:17]=[CH:18][N:19]=2)[CH:16]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 4593OlprinoneHCID 12896473Azane;hydrate

Produkt 1

HCID 138523301,2-Dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-pyridineAusbeute 44,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1004Phosphoric AcidLösungsmittel

Versuchsvorschrift

In 10 ml of 85% phosphoric acid was refluxed 1 g of 1,2-dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-3-pyridinecarbonitrile for 18 hours. After cooling, water was added and then conc. ammonia water was further added to the reaction mixture to render the mixture alkaline. The mixture was extracted with chloroform. After washing with water and drying over magnesium sulfate, chloroform was removed by distillation under reduced pressure. The residue was recrystallized from ethanol-ether to obtain 0.4 g of 1,2-dihydro-6-methyl-5-(imidazo[1,2-a]pyridin-6-yl)-2-oxo-pyridine.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionThe mixture was extracted with chloroform
  3. washAfter washing with water
  4. dry with materialdrying over magnesium sulfate, chloroform
  5. customwas removed by distillation under reduced pressure
  6. customThe residue was recrystallized from ethanol-ether

Quellen und Nachweise

ORD-Eintrag
ord-deaf50ac95c54fa5b029f10b0eaf4181
Quelldatensatz
uspto-grants-1988_12
Patentnummer
US04791202

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