反应详情

温度

25 °C

Oxalyl chloride (15 mL) was added dropwise at 0° C. to a suspension of 3-bromo-6-fluoro-2-methoxybenzoic acid (15 g, 60 mmol) in 100 mL of DCM with 0.5 mL of DMF. The mixture was stirred at 25° C. for 2 hours and the clear solution was concentrated to dryness under reduced pressure. The residue dissolved in 60 mL of anhydrous acetonitrile was added to 600 mL of aqueous NH3.H2O at 0° C. and stirred for 2 hours, then filtered to give 3-bromo-6-fluoro-2-methoxybenzamide.

1. concentrationthe clear solution was concentrated to dryness under reduced pressure
2. dissolutionThe residue dissolved in 60 mL of anhydrous acetonitrile
3. additionwas added to 600 mL of aqueous NH3.H2O at 0° C.
4. stirringstirred for 2 hours
5. filtrationfiltered