872624-52-7

61500-87-6

872624-52-7

Step 3: Preparation of methyl 2-amino-5-iodo-4-(trifluoromethyl)benzoate; A solution of methyl 2-amino-4-(trifluoromethyl)benzoate (178 g, 812 mmol) in ethanol (3.3 L) was slowly added to a suspension in ethanol (5 L) containing iodine (206.1 g, 812 mmol) and silver(II) sulfate (253 g, 812 mmol). . The reaction was stirred at room temperature and under nitrogen protection for 2 hours. After completion of the reaction, the reaction mixture was filtered through a diatomaceous earth pad and the pad was washed with ethanol (2 L). The filtrate and washings were combined and concentrated under reduced pressure at 40°C to remove the solvent. The resulting residue was dissolved in ethyl acetate (7.5 L) and washed sequentially with saturated sodium bicarbonate solution (3 x 1.5 L), water (3 x 1.5 L) and brine (2 L). The organic phase was dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to afford methyl 2-amino-5-iodo-4-(trifluoromethyl)benzoate as a light brown crystalline solid (276.0 g, 99% yield).