Hydrochloric Acid → 2-Pyridin-2-yl-4-(6-trifluormethylpyridin-3-yl)-1,2-dihydro-3h-pyrazol-3-one

HRID 1526089Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1526089
C(O[C:4](=[O:18])[C:5]([C:8]1[CH:9]=[N:10][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:12][CH:13]=1)=[CH:6]O)C.[NH:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1)[NH2:20].C([O-])C.[Na+].Cl>C(O)C>[N:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[N:19]1[C:4](=[O:18])[C:5]([C:8]2[CH:9]=[N:10][C:11]([C:14]([F:15])([F:16])[F:17])=[CH:12][CH:13]=2)=[CH:6][NH:20]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 786452-HydrazinopyridineHCID 2723922Sodium ethoxideHCID 687048893-Hydroxy-2-(6-trifluoromethylpyridin-3-yl)-acrylic acid ethyl ester

Produkt 1

HCID 591869752-Pyridin-2-yl-4-(6-trifluormethylpyridin-3-yl)-1,2-dihydro-3h-pyrazol-3-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

261 mg (1.00 mmol) of the compound from Example 41A and 115 mg (1.05 mmol) 2-hydrazinopyridine are dissolved in 5 ml anhydrous ethanol under argon and the mixture is stirred at RT for 20 h. 68 mg (1.00 mmol) sodium ethanolate are added, the mixture is stirred at RT for 30 min and 1 M hydrochloric acid and a little ethanol are then added, a precipitate separating out. This is filtered off, washed with a little ethanol and dried in vacuo.

Aufarbeitung

  1. stirringthe mixture is stirred at RT for 30 min
  2. customa precipitate separating out
  3. filtrationThis is filtered off
  4. washwashed with a little ethanol
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-e6e2cc5e18654ff9b82927e2656b93b3
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09085572B2

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