467435-07-0

445-13-6

467435-07-0

The general procedure for the synthesis of 4-bromo-2-chlorobenzotrifluoride using 4-amino-2-chlorobenzotrifluoride as starting material was as follows: 4-amino-2-chlorobenzotrifluoride (9.780 g; 50.007 mmol) was dissolved in acetonitrile (65 mL), and copper(II) bromide (11.169 g; 50.007 mmol) was added to form a green, non-homogeneous mixture. The mixture was heated to 45°C. Subsequently, a solution of tert-butyl nitrite (6.53 mL; 55.008 mmol) in acetonitrile (10 mL) was added slowly and dropwise over 30 minutes. After the dropwise addition, the reaction mixture was continued to be stirred at 45°C for 2 hours. Upon completion of the reaction, the dark, inhomogeneous mixture was cooled to room temperature and purified directly by fast column chromatography (dichloromethane as eluent). After concentration under reduced pressure to remove the solvent, the target product, 4-bromo-2-chloro-1-trifluoromethylbenzene, was obtained as a yellow oil (12.820 g; 50% yield).LC-MS analysis: retention time t R = 1.10 min; [M + H]+: no ionization peak was observed.