Reaktion #45832

Reaktionsgleichung

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

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compound

Ausbeute 97.3%

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

Ausbeute 97.3%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle