Sodium Bisulfate → 2-(2-trifluoromethyl-phenyl)-3H-pyrido[2,3-d]pyrimidin-4-one

HRID 38173

Reaktionsgleichung

Reaktionsgleichung von HRID 38173
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[C:5]([NH:7][C:8]1[N:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10]([NH2:12])=[O:11])=O.[O-]CC.[K+].S([O-])(O)(=O)=O.[Na+]>C(O)C.O>[F:1][C:2]([F:22])([F:21])[C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[C:5]1[NH:12][C:10](=[O:11])[C:9]2[CH:13]=[CH:14][CH:15]=[N:16][C:8]=2[N:7]=1

Komponenten

6

Edukt 3

HCID 516919Sodium BisulfateHCID 219392142-[2-(Trifluoromethyl)benzamido]pyridine-3-carboxamideHCID 23670592Potassium ethoxide

Produkt 1

HCID 1358508342-(2-trifluoromethyl-phenyl)-3H-pyrido[2,3-d]pyrimidin-4-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

2-(2-Trifluoromethyl-benzoylamino)-nicotinamide (800 mg, 2.6 mmol) is dissolved in 10 ml of ethanol. Potassium ethoxide (435 mg, 5.2 mmol) is added to the solution which is heated to reflux for 16 h. The reaction mixture is evaporated in vacuo to afford a gummy residue that is dissolved in water and acidified with 10% sodium hydrogen sulfate to pH 7. The resulting precipitate is filtered and dried under vacuum at 50 C to give 2-(2-trifluoromethyl-phenyl)-3H-pyrido[2,3-d]pyrimidin-4-one.

Aufarbeitung

  1. temperatureis heated
  2. temperatureto reflux for 16 h
  3. customThe reaction mixture is evaporated in vacuo
  4. customto afford a gummy residue that
  5. filtrationThe resulting precipitate is filtered
  6. customdried under vacuum at 50 C

Quellen und Nachweise

ORD-Eintrag
ord-021814edc3f74ffab715b58d6995521d
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524720B2

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