4-BROMO-2,3-DIFLUOROANILINE synthesis

Yield:112279-72-8 100%

Reaction Conditions:

with N-Bromosuccinimide in N,N-dimethyl-formamide for 1 h;Cooling with ice;

Steps:

14
To a solution of 2,3-difluoroaniline (G-1) (38.0 ml, 375 mmol) in anhydrous dimethylformamide (20 ml) was added NBS (70.1 g, 394 mmol) with ice-cooling, then the reaction mixture was stirred for 1 hour. To the reaction solution was added water, then the reaction solution was extracted with ethyl acetate. The extraction was washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to give Compound (G-2) (81.9 g, quant.) as an oil.Compound (G-2);Method C: Rt=1.81 min, 207.65 (ES+)

References:

Shionogi & Co., Ltd. US2012/253040, 2012, A1 Location in patent:Page/Page column 35

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