Реакция #2075715

Уравнение реакции

Tin (II) chloride dihydrate

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

sodium bicarbonate

→

title compound

Выход 73.9%

4-Chloro-2,5-difluorophenylamine

Выход 73.9%

Растворители

ethyl acetate

Условия реакции

Обработка

1. 1
   Экстракцияextracted with ethyl acetate
2. 2
   ПромывкаThe organic phase was washed several more times with water
3. 3
   Другоеdried
4. 4
   Фильтрацияfiltered
5. 5
   Концентрированиеconcentrated
6. 6
   Другоеpurified by flash chromatography on silica gel (hexane/diethyl ether)

Методика

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).

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