Yield:874784-14-2 82%

Reaction Conditions:

with N-Bromosuccinimide in dichloromethane at 0 - 20; for 1 h;

Steps:

1.1 Step 1 : 2-amino-5-bromo-3-fluoro-benzoic acid

2-Amino-3-fluoro-benzoic acid (2.00 g, 12.9 mmol) was suspended in dichloromethane (34.0 mL) and N-bromosuccinimide (2.39 g, 12.9 mmol) was added in small portions at 0 °C. The reaction mixture was stirred at room temperature for 1 hour. The reaction mixture was filtered and the solid was washed with dichloromethane (30 mL) and dried in air for 15 min to give the desired product as a white solid (2.46 g, 10.5 mmol, 82% Yield). LCMS: 0.82 min; ES+ 234/236 ( M+H+); ^XH NMR (DMSO-d₆, 400MHz): δ (ppm) 7.62-7.66 (s, 1H), 7.52 (d, 1H).

References:

WO2018/17490,2018,A1 Location in patent:Paragraph 0153; 0154