Methylamine → Pyrido(2,3-d)pyrimidine-2,4(1H,3H)-dione, 1,3-dimethyl-5-(methylamino)-

HRID 1382720Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1382720
Cl[C:2]1[C:11]2[C:10](=[O:12])[N:9]([CH3:13])[C:8](=[O:14])[N:7]([CH3:15])[C:6]=2[N:5]=[CH:4][CH:3]=1.[CH3:16][NH2:17]>CN(C=O)C>[CH3:16][NH:17][C:2]1[C:11]2[C:10](=[O:12])[N:9]([CH3:13])[C:8](=[O:14])[N:7]([CH3:15])[C:6]=2[N:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 143046845-Chloro-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

Produkt 1

HCID 3086957Pyrido(2,3-d)pyrimidine-2,4(1H,3H)-dione, 1,3-dimethyl-5-(methylamino)-Ausbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

0.4 g of Compound 1 and 1.86 g of methylamine (30% methanol solution) were added to 10 ml of DMF. The solution was stirred 2 hr at room temperature and the solvent was distilled off under reduced pressure. After adding water, the resulting crude crystals were separated by filtration and recrystallized from ethyl acetate to give 0.23 g of 5-methylamino-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4-dione (Compound 7)

Aufarbeitung

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionAfter adding water
  3. customthe resulting crude crystals were separated by filtration
  4. customrecrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-2c22c547a15740af85438460200dcb28
Quelldatensatz
uspto-grants-1989_02
Patentnummer
US04808587

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