1-Bromo-4-chloro-2-(difluoromethoxy)benzene synthesis

Yield:1056942-37-0 98%

Reaction Conditions:

with caesium carbonate in water;N,N-dimethyl-formamide at 100; for 4 h;

Steps:

27 4-chloro-2-(difluoromethoxy)bromobenzene

To a solution of 2-bromo-5-chlorophenol (1 g, 4.8 mmol) in DMF/water (45 mL/5 mL) was added sodium chlorodifluoroacetate (1.95 g, 12.0 mmol) and cesium carbonate (3.14 g, 9.64 mmol), and the reaction mixture was heated to 100° C. for 4 hours.
The reaction mixture was cooled and diluted with TBME (20 mL) and water (20 mL).
The organic layer was collected, washed with saturated aqueous NaHCO₃ solution, brine, dried over Na₂SO₄ and concentrated in vacuo to afford the title compound (1.21 g, 98%), which was used without further purification.

References:

US2014/315878,2014,A1 Location in patent:Paragraph 0493; 0494