반응 #472326

반응 방정식

3-formyl-4-methoxy-5-trifluoromethoxybenzoic acid

hydroxylamine hydrochloride

→

title compound

수율 95.2%

3-cyano-4-methoxy-5-trifluoromethoxybenzoic acid

수율 95.2%

용매

formic acid

반응 조건

후처리

1. 1
   온도the mixture was refluxed for 16 hours
2. 2
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure and 1N hydrochloric acid
3. 3
   workup.ADDITIONwas added
4. 4
   추출the mixture was extracted with ethyl acetate
5. 5
   세척The organic layer was washed with saturated brine
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

실험 절차

3-formyl-4-methoxy-5-trifluoromethoxybenzoic acid (4.22 g) was dissolved in formic acid (20 mL), and hydroxylamine hydrochloride (1.22 g) was added to the solution, and then the mixture was refluxed for 16 hours. The solvent was distilled off under reduced pressure and 1N hydrochloric acid 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 (3.97 g) as a brown solid.

출처