N-bromobutanimide → 5-Bromo-2-hydroxy-3-(trifluoromethoxy)benzaldehyde

HRID 385141ノート

反応式

HRID 385141 の反応式
[OH:1][C:2]1[C:9]([O:10][C:11]([F:14])([F:13])[F:12])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[Br:15]N1C(=O)CCC1=O>ClCCl>[Br:15][C:7]1[CH:8]=[C:9]([O:10][C:11]([F:12])([F:13])[F:14])[C:2]([OH:1])=[C:3]([CH:6]=1)[CH:4]=[O:5]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 27792702-Hydroxy-3-(trifluoromethoxy)benzaldehyde

生成物 1

HCID 27792795-Bromo-2-hydroxy-3-(trifluoromethoxy)benzaldehyde収率 99.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-hydroxy-3-trifluoromethoxybenzaldehyde (10.38 g) was dissolved in dichloromethane (100 mL), and N-bromosuccinimide (9.41 g) was added to the solution, and then the mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 10% sodium thiosulfate and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (14.27 g) as a brown solid.

後処理

  1. distillationThe solvent was distilled off under reduced pressure and water
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with 1N hydrochloric acid, 10% sodium thiosulfate and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-79854c2cfc0244569810b1151a8142f4
出典データセット
uspto-grants-2013_02
特許番号
US08367843B2

反応ノート

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