Reacción #2075715

Ecuación de reacción

Tin (II) chloride dihydrate

1-chloro-2,5-difluoro-4-nitrobenzene

sodium bicarbonate

→

title compound

Rendimiento 73.9%

4-Chloro-2,5-difluorophenylamine

Rendimiento 73.9%

Disolventes

ethyl acetate

Condiciones de reacción

Tratamiento posterior

1. 1
   Extracciónextracted with ethyl acetate
2. 2
   LavadoThe organic phase was washed several more times with water
3. 3
   Otrodried
4. 4
   Filtraciónfiltered
5. 5
   Concentraciónconcentrated
6. 6
   Otropurified by flash chromatography on silica gel (hexane/diethyl ether)

Procedimiento

Tin (II) chloride dihydrate (15.5 g, 68.7 mmol) was dissolved in ethyl acetate (50 mL) and 1-chloro-2,5-difluoro-4-nitrobenzene (2.65 g, 13.7 mmol) was added dropwise. The reaction mixture was then stirred at 70° C. for 1 h. The reaction mixture was then carefully added to saturated aqueous sodium bicarbonate and then extracted with ethyl acetate. The organic phase was washed several more times with water, dried, filtered, concentrated and purified by flash chromatography on silica gel (hexane/diethyl ether) to give the title compound as a white solid (1.65 g, 73.9% yield): 1H NMR (CDCl3): δ 7.02 (dd, 1H), 6.57 (dd, 1H), 3.81 (br s, 2H).

Fuente