Water → Pyridine, 2-methoxy-4-(trifluoromethyl)-

HRID 242424Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 242424
Cl[C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=1.[CH3:12][O-:13].[Na+].O>CO>[F:9][C:8]([F:11])([F:10])[C:6]1[CH:5]=[CH:4][N:3]=[C:2]([O:13][CH3:12])[CH:7]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 1449582-Chloro-4-(trifluoromethyl)pyridineHCID 10942334Sodium Methoxide

Produkt 1

HCID 18539797Pyridine, 2-methoxy-4-(trifluoromethyl)-Ausbeute 85,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution having 5.05 g (27.8 mmol) of 2-chloro-4-trifluoromethylpyridine and 3.59 g (66.5 mmol) of sodium methoxide dissolved in 40 ml of methanol was stirred under reflux with heating for 4 hours. Water was added to terminate the reaction, followed by extraction with diethyl ether. The organic layer was dried over anhydrous sodium sulfate and subjected to filtration on the pad of a silica gel cake. The solvent was distilled off under reduced pressure to obtain 4.19 g (yield: 85%) of 4-trifluoromethyl-2-methoxypyridine.

Aufarbeitung

  1. temperatureunder reflux
  2. temperaturewith heating for 4 hours
  3. customto terminate
  4. customthe reaction
  5. extractionfollowed by extraction with diethyl ether
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. filtrationsubjected to filtration on the pad of a silica gel cake
  8. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-767f5c5bf6d3402399794a24f7890bb9
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08653113B2

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