Reaktion #472197

Reaktionsgleichung

3-formyl-4-methoxy-5-trifluoromethylbenzoic acid

hydroxylamine hydrochloride

→

title compound

Ausbeute 27.2%

3-cyano-4-methoxy-5-trifluoromethylbenzoic acid

Ausbeute 27.2%

Lösungsmittel

formic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was refluxed for 19 hours
2. 2
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure and water
3. 3
   workup.ADDITIONwas added
4. 4
   Extraktionthe mixture was extracted with ethyl acetate
5. 5
   WaschenThe organic layer was washed with saturated brine
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

3-formyl-4-methoxy-5-trifluoromethylbenzoic acid (58.04 g) was dissolved in formic acid (290 mL), and hydroxylamine hydrochloride (17.07 g) was added to the solution, and the mixture was refluxed for 19 hours. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (15.62 g) as a brown solid.

Quelle