Reaktion #582835

Reaktionsgleichung

hydrochloric acid

ethyl 4-bromo-2-nitro-6-(trifluoromethyl)phenylcarbamate

potassium carbonate

3-trifluoromethylbenzyl bromide

→

title compound

Ausbeute 82.0%

ethyl 4-bromo-2-nitro-6-(trifluoromethyl)phenyl[3-(trifluoromethyl)benzyl]carbamate

Ausbeute 82.0%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted with ethyl acetate
2. 2
   WaschenThe organic layer was washed with 1N hydrochloric acid, saturated brine, saturated aqueous sodium bicarbonate solution
3. 3
   Trocknensaturated brine, dried over anhydrous magnesium sulfate
4. 4
   Einengenconcentrated in vacuo
5. 5
   SonstigeThe resultant residue was purified by silica gel column (35 g, hexane:ethyl acetate=20:1)

Vorschrift

To a solution of ethyl 4-bromo-2-nitro-6-(trifluoromethyl)phenylcarbamate (275.3 mg) and potassium carbonate (108.3 mg) in N,N-dimethylformamide (5 ml) was added 3-trifluoromethylbenzyl bromide (0.180 ml). After the mixture was stirred at room temperature for 1 hour, 1N hydrochloric acid (ca. 30 ml) was added and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, saturated brine, saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (35 g, hexane:ethyl acetate=20:1) to give the title compound (345.3 mg, 82%).

Quelle