반응 #160530

반응 방정식

water

dimethyl-(4-nitro-2-trifluoromethylphenyl)amine

(4-chlorophenoxy)acetonitrile

potassium tert-butoxide

→

title compound

수율 9.9%

(5-Dimethylamino-2-nitro-4-trifluoromethylphenyl)acetonitrile

수율 9.9%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   추출this mixture was extracted with ethyl acetate
2. 2
   세척This organic layer was washed with water and brine
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   기타The solvent was removed under reduced pressure
5. 5
   기타The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate)

실험 절차

To a solution of dimethyl-(4-nitro-2-trifluoromethylphenyl)amine (0.95 g) in N,N-dimethylformamide (20 mL) were added (4-chlorophenoxy)acetonitrile (0.75 g) and 1 mol/L potassium tert-butoxide (4.5 mL, in tetrahydrofuran solution) under ice cooling, and this mixture was stirred at the same temperature for 1 hour. This reaction mixture was poured into water, and this mixture was extracted with ethyl acetate. This organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (0.11 g).

출처