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

HRID 1912265Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1912265
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

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-ef417b3050c7492ba7de4fbd179ff0db
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08609150B2

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