Реакция #1055525

Уравнение реакции

2-fluoro-5-nitrobenzonitrile

→

4-fluoro-3-cyanoaniline

Выход 85.4%

Растворители

ethylacetate

Условия реакции

Обработка

1. 1
   Температураto reflux for 1.5 h
2. 2
   Температураto cool
3. 3
   ДругоеThe mixture was partitioned between ethyl acetate and sodium bicarbonate (sat. in water)
4. 4
   ЭкстракцияThe aqueous phase was extracted with ethyl acetate four times
5. 5
   ПромывкаThe organic phase was washed with 4×H2O
6. 6
   Сушкаdried over sodium sulfate
7. 7
   Фильтрацияfiltered
8. 8
   Концентрированиеconcentrated

Методика

To a solution of 2-fluoro-5-nitrobenzonitrile (2.0 g) in ethylacetate (50 mL) was added stannous chloride dihydrate (27.0 g). The mixture was brought to reflux for 1.5 h and allowed to cool. The mixture was partitioned between ethyl acetate and sodium bicarbonate (sat. in water). The aqueous phase was extracted with ethyl acetate four times. The organic phase was washed with 4×H2O, dried over sodium sulfate, filtered and concentrated to leave 4-fluoro-3-cyanoaniline (1.40 g). CI mass spectrum z (rel. intensity) 137 (M+H, 100).

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