Réaction #45832

Équation de réaction

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

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compound

Rendement 97.3%

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

Rendement 97.3%

Solvants

N,N-dimethylformamide

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source