Реакция #45832

Уравнение реакции

4-amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methyl-5-nitrobiphenyl-3-carbonitrile

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compound

Выход 97.3%

4,5-Diamino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methylbiphenyl-3-carbonitrile

Выход 97.3%

Растворители

N,N-dimethylformamide

Условия реакции

Обработка

1. 1
   ДругоеThe insoluble matter was removed by filtration under suction
2. 2
   workup.ADDITIONthe filtrate was diluted with ethyl acetate
3. 3
   Промывкаwashed with aqueous saturated sodium carbonate solution and saturated brine in that order
4. 4
   Сушкаdried over anhydrous sodium sulfate
5. 5
   ДругоеThe solvent was evaporated away under reduced pressure
6. 6
   Другоеby drying with a vacuum pump

Методика

An aqueous solution (14 ml) of iron chloride hexahydrate (0.83 g, 3.06 mmol) and zinc (5.01 g, 76.6 mmol) were added to an N,N-dimethylformamide (35 ml) solution of 4-amino-6-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-2-methyl-5-nitrobiphenyl-3-carbonitrile (I-268) (1.40 g, 3.83 mmol), followed by stirring at room temperature for 1 hour. The insoluble matter was removed by filtration under suction, then the filtrate was diluted with ethyl acetate, washed with aqueous saturated sodium carbonate solution and saturated brine in that order, and dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, followed by drying with a vacuum pump to obtain the entitled compound (1.25 g, 97%) as a dark brown solid.

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