Dimethylformamide dimethyl acetal → HCID 53948848, Verbindung

HRID 476914Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 476914
[NH2:1][C:2]1[N:7]([CH3:8])[C:6](=[O:9])[N:5]([CH3:10])[C:4](=[O:11])[C:3]=1[C:12]#[N:13].CO[CH:16](OC)[N:17]([CH3:19])[CH3:18]>CN(C)C=O>[C:12]([C:3]1[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[N:7]([CH3:8])[C:2]=1[N:1]=[CH:16][N:17]([CH3:19])[CH3:18])#[N:13]

Komponenten

4

Edukt 2

HCID 78373Dimethylformamide dimethyl acetalHCID 13296989HCID 13296989, Verbindung

Produkt 1

HCID 53948848HCID 53948848, VerbindungAusbeute 99,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

3.6 g (20 mmol) of 6-amino-5-cyano-1,3-dimethyluracil and 9.36 g (80 mmol) of dimethylformamide dimethyl acetal were added to 36 ml of dimethylformamide, and the reaction mixture was refluxed for 30 minutes. The solvent was removed by distillation under reduced pressure. The crude product was crystallized from ether, filtered off, and recrystallized from ethyl acetate to give 4.68 g of 5-cyano-6-dimethylaminomethyleneamino-1,3-dimethyluracil (compound 15) in a 99% yield.

Aufarbeitung

  1. temperaturethe reaction mixture was refluxed for 30 minutes
  2. customThe solvent was removed by distillation under reduced pressure
  3. customThe crude product was crystallized from ether
  4. filtrationfiltered off
  5. customrecrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-37c1a83c9479454b8ae0f8c0d0b09c13
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04886807

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