2,4-DIBROMO-6-FLUOROBENZOYL CHLORIDE synthesis

Yield:-

Reaction Conditions:

with oxalyl dichloride;N,N-dimethyl-formamide in tetrahydrofuran;dichloromethane at 20; for 1 h;

Steps:

10.B

Part B. 2,4-Dibromo-6-fluorobenzamide To a solution of the product from step A (14.14 g, 47.77 mmol) in THF (50 mL) and dichloromethane (70 mL) was sequentially added oxalyl chloride (4.85 mL, 57.32 mmol) and DMF (10 drops). The reaction mixture stirred at RT for 1 h, concentrated, the residue was dissolved in dichloromethane (10 mL) and slowly added to an ice cold solution of 7N ammonia in methanol (350 mL). The reaction mixture was stirred at RT for 1 h, concentrated, dissolved in ethyl acetate and washed with water. The organic layer was dried over sodium sulfate and concentrated to give the title compound as a brown solid (11.74 g, 83% yield).

References:

US2006/178386,2006,A1 Location in patent:Page/Page column 20