Bromine → HCID 178519632、化合物

HRID 913820ノート

反応式

HRID 913820 の反応式
[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]=1

参加物

5

反応物 2

HCID 24408BromineHCID 575462105-(trifluoromethyl)-1H-indazole-7-carbaldehyde

生成物 1

HCID 178519632HCID 178519632、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6344Dichloromethane溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-8903e6478d4843a4aa5885914fe41c70
出典データセット
uspto-grants-2011_09
特許番号
US08026257B2

反応ノート

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