反应详情

To a mixture of 5-(trifluoromethyl)-1H-indazole-7-carbaldehyde (270 mg, 1.26 mmol) in acetic acid (5 mL) was added bromine (97 μL, 1.89 mmol) slowly over 5 min. After 1 h, the reaction mixture was diluted with methylene chloride, washed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×), brine (2×), dried over sodium sulfate, and concentrated to afford 340 mg (92%) as a yellow powder. 1H-NMR (CDCl3, 300 MHz) δ 10.18 (s, 1H), 8.22 (s, 1H), 8.15 (s, 1H). Mass spec.: 294.81 (MH)+.

1. washwashed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×), brine (2×)
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated
4. customto afford 340 mg (92%) as a yellow powder