Bromine → HCID 178519632, 화합물
반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]2[C:9](=[C:10]([CH:12]=[O:13])[CH:11]=1)[NH:8][N:7]=[CH:6]2.[Br:16]Br>C(O)(=O)C.C(Cl)Cl>[Br:16][C:6]1[C:5]2[C:9](=[C:10]([CH:12]=[O:13])[CH:11]=[C:3]([C:2]([F:1])([F:14])[F:15])[CH:4]=2)[NH:8][N:7]=1참가 물질
5
실험 절차
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)+.
후처리
- washwashed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×), brine (2×)
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customto afford 340 mg (92%) as a yellow powder
출처 및 근거
- ORD 기록
- ord-8903e6478d4843a4aa5885914fe41c70
- 출처 데이터셋
- uspto-grants-2011_09
- 특허 번호
- US08026257B2
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