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

HRID 385141노트

반응식

HRID 385141 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-79854c2cfc0244569810b1151a8142f4
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367843B2

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