Yield:-

Reaction Conditions:

with bromine in methanol; for 1.5 h;

Steps:

I

To 3-chloro-4-amino-benzonitrile (5 g, 32.9 mmol) in Methanol (80 mL) was added dropwise bromine (5.3 g, 33.1 mmol) in Methanol (20 mL). The mixture was stirred for 1.5 hours. Solvent was removed by rotovap and resulting solid was dried in vacuum. 3-Chloro-4-amino-5-bromobenzonitrile was obtained as a white solid. ¹H NMR (300 MHz, CD₃OD): δ7.63 (s, 1H), 7.75 (s, 1H). MH⁺=230.97, 232.97.

References:

US2006/287287,2006,A1 Location in patent:Page/Page column 19