Potassium Carbonate → 4H-1,3,4-Oxadiazin-5(6H)-one, 2-(2,6-dimethylimidazo(1,2-a)pyridin-3-yl)-

HRID 986386Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 986386
Cl[CH2:2][C:3]([NH:5][NH:6][C:7]([C:9]1[N:13]2[CH:14]=[C:15]([CH3:18])[CH:16]=[CH:17][C:12]2=[N:11][C:10]=1[CH3:19])=[O:8])=[O:4].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C.CN(C)C=O>[CH3:19][C:10]1[N:11]=[C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][N:13]2[C:9]=1[C:7]1[O:8][CH2:2][C:3](=[O:4])[NH:5][N:6]=1

Komponenten

5

Edukt 2

HCID 11430Potassium CarbonateHCID 14032941HCID 14032941, Verbindung

Produkt 1

HCID 30653094H-1,3,4-Oxadiazin-5(6H)-one, 2-(2,6-dimethylimidazo(1,2-a)pyridin-3-yl)-Ausbeute 16,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 6569Methyl Ethyl KetoneLösungsmittel

Versuchsvorschrift

A mixture of 21 g of N'-chloroacetyl-2,6-dimethylimidazo[1,2-a]pyridine-3-carbohydrazide and 30 g of potassium carbonate in 200 ml of methyl ethyl ketone and 100 ml of dimethylformamide is stirred with refluxing for 5 hours. After insoluble substances are filtered off, the solvent is distilled off and water is added to the resultant residue. The precipitated crystals are collected by filtration and recrystallized from methanol to give 3 g of 2-(2,6-dimethylimidazo[1,2-a]pyridin-3-yl)-4,6-dihydro-1,3,4-oxadiazin-5-one as white crystals, melting at 313° C. with decomposition.

Aufarbeitung

  1. temperaturewith refluxing for 5 hours
  2. filtrationAfter insoluble substances are filtered off
  3. distillationthe solvent is distilled off
  4. additionwater is added to the resultant residue
  5. filtrationThe precipitated crystals are collected by filtration
  6. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-c3f4f0b9ac544bca8fd260158c94a46c
Quelldatensatz
uspto-grants-1987_12
Patentnummer
US04713381

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