Sodium Hydroxide → 3-Bromo-5-hydroxybenzoic acid

HRID 416963

반응식

HRID 416963 반응식
[OH-:1].[Na+].[Br:3][C:4]1[CH:5]=[C:6]([CH:10]=[C:11](I)[CH:12]=1)[C:7]([OH:9])=[O:8]>O>[Br:3][C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([OH:1])[CH:12]=1)[C:7]([OH:9])=[O:8]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 51825203-Bromo-5-iodobenzoic acid

생성물 1

HCID 157355113-Bromo-5-hydroxybenzoic acid수율 93%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

To a solution of NaOH (12.2 g; 305.8 mmol) in 300 mL of water was added 3-bromo-5-iodo-benzoic acid (20 g, 61.2 mmol) and Cu2O (866 mg, 6.1 mmol). The reaction mixture was heated at 100° C. for 24 h. After complete consumption of the starting material, the reaction mixture was cooled to room temperature and filtered through Celite™. The filtrate was then acidified with 10% aq. HCl and extracted into ethyl acetate. The organic extract was dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford the title compound as a tan solid (12.3 g, 93% yield). HR-ES (−) calcd for C7HSO3Br [M−H]− 214.9349, observed 214.9350

후처리

  1. customAfter complete consumption of the starting material
  2. temperaturethe reaction mixture was cooled to room temperature
  3. filtrationfiltered through Celite™
  4. extractionextracted into ethyl acetate
  5. extractionThe organic extract
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b4614be5f9334b0e854fa6f0a5f2d44b
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088936B2

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