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2-Trifluoromethyl-4-(1-hydroxyethyl)-7-methoxy-pyrazolo[1,5-a]pyridine → 4-Acetyl-2-trifluoromethyl-7-methoxy-pyrazolo[1,5-a]pyridine

HRID 2357909
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2357909
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:16]=[C:6]2[C:7]([CH:13]([OH:15])[CH3:14])=[CH:8][CH:9]=[C:10]([O:11][CH3:12])[N:5]2[N:4]=1>ClCCl.[O-2].[O-2].[Mn+4]>[C:13]([C:7]1[C:6]2[N:5]([N:4]=[C:3]([C:2]([F:1])([F:18])[F:17])[CH:16]=2)[C:10]([O:11][CH3:12])=[CH:9][CH:8]=1)(=[O:15])[CH3:14]
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Komponenten

4

Edukt 1

HCID 593893232-Trifluoromethyl-4-(1-hydroxyethyl)-7-methoxy-pyrazolo[1,5-a]pyridine

Produkt 1

HCID 593893454-Acetyl-2-trifluoromethyl-7-methoxy-pyrazolo[1,5-a]pyridineAusbeute 66,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418406HCID 178418406, VerbindungKatalysator4×HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

The compound of Example 134 (1.64 g) was dissolved in dichloromethane (30.0 mL). To this solution, activated manganese dioxide (5.48 g) was added and the mixture was stirred at room temperature for 16 hours. Subsequently, a second portion of activated manganese dioxide (5.48 g) was added and the mixture was stirred at room temperature for 10 hours. A third portion of activated manganese dioxide (5.48 g) was then added and the mixture was stirred at room temperature for 10.5 hours. Finally, a fourth portion of activated manganese dioxide (2.74 g) was added and the mixture was stirred for 13.5 hours. Subsequently, the reaction mixture was filtered through Celite and the filtrate was evaporated to afford the title compound as a pale yellow powder (1.08 g).

Aufarbeitung

  1. additionwas added
  2. stirringthe mixture was stirred at room temperature for 10 hours
  3. stirringthe mixture was stirred at room temperature for 10.5 hours
  4. stirringthe mixture was stirred for 13.5 hours
  5. filtrationSubsequently, the reaction mixture was filtered through Celite
  6. customthe filtrate was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-b3886fbdbb674471b20ea1513c25a78b
Quelldatensatz
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07763617B2

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