反应 #45832

反应方程式

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

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compound

收率 97.3%

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

收率 97.3%

溶剂

N,N-dimethylformamide

反应条件

后处理

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

实验过程

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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