Ethyl Acetate → 2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 2300059Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2300059
CS([C:4]1[N:5]=[CH:6][C:7]2[CH:13]=[CH:12][C:11](=[O:14])[NH:10][C:8]=2[N:9]=1)=O.CS(C1N=C[C:22]2[CH:28]=[CH:27][C:26](=O)[NH:25][C:23]=2N=1)(=O)=O.[C:30](OCC)(=O)C>NC1C=CC=CC=1>[C:23]1([NH:25][C:4]2[N:5]=[CH:6][C:7]3[CH:13]=[CH:12][C:11](=[O:14])[NH:10][C:8]=3[N:9]=2)[CH:22]=[CH:28][CH:27]=[CH:26][CH:30]=1

Komponenten

5

Edukt 3

HCID 8857Ethyl AcetateHCID 106084702-(Methylsulfinyl)pyrido[2,3-d]pyrimidin-7(1H)-oneHCID 183749342-(Methylsulfonyl)pyrido[2,3-d]pyrimidin-7(1H)-one

Produkt 1

HCID 105140732-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6115AnilineLösungsmittel

Versuchsvorschrift

A suspension of 204 mg of the mixture of 2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one and 2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one in 1 mL of aniline was heated at reflux for 10 minutes resulting in a dark brown solution. Upon cooling to room temperature, a solid formed. Ethyl acetate was added, and the solid was collected by filtration, washed with ethyl acetate, then suspended in methanol and filtered, and washed with additional methanol to provide 175 mg of 2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one, mp>350° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 10 minutes
  3. customresulting in a dark brown solution
  4. customa solid formed
  5. filtrationthe solid was collected by filtration
  6. washwashed with ethyl acetate
  7. filtrationfiltered
  8. washwashed with additional methanol

Quellen und Nachweise

ORD-Eintrag
ord-046426131380437b96579baa59856a8a
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06498163B1

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