تفاعل #2075715

معادلة التفاعل

Tin (II) chloride dihydrate

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

sodium bicarbonate

→

title compound

المردود 73.9%

4-Chloro-2,5-difluorophenylamine

المردود 73.9%

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with ethyl acetate
2. 2
   غسيلThe organic phase was washed several more times with water
3. 3
   أخرىdried
4. 4
   ترشيحfiltered
5. 5
   تركيزconcentrated
6. 6
   أخرىpurified by flash chromatography on silica gel (hexane/diethyl ether)

الإجراء التجريبي

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).

المصدر