Water → 4,5-Dinitrobenzene-1,2-diol

HRID 483364노트

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HRID 483364 반응식
C[O:2][C:3]1[C:8]([O:9]C)=[CH:7][C:6]([N+:11]([O-:13])=[O:12])=[C:5]([N+:14]([O-:16])=[O:15])[CH:4]=1.O>Br>[OH:2][C:3]1[C:8]([OH:9])=[CH:7][C:6]([N+:11]([O-:13])=[O:12])=[C:5]([N+:14]([O-:16])=[O:15])[CH:4]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 2229891,2-Dimethoxy-4,5-dinitrobenzene

생성물 1

HCID 141714294,5-Dinitrobenzene-1,2-diol수율 79.5%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

10 g (44 mmol) of 4,5-dimethoxy-1,2-dinitrobenzene was suspended in 150 ml of 45% hydrobromic acid, and the suspension was refluxed at a boiling point for 6 hours. The reaction solution was allowed to cool to room temperature, and 500 ml of water was added thereto. The mixture was extracted three times with ethyl acetate. The organic layer was washed with a 10% sodium bicarbonate aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The crystal residue was washed with methylene chloride to obtain 7 g (yield: 79%) of 4,5-dihydroxy1,2-dinitrobenzene.

후처리

  1. temperaturethe suspension was refluxed at a boiling point for 6 hours
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washThe organic layer was washed with a 10% sodium bicarbonate aqueous solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. washThe crystal residue was washed with methylene chloride

출처 및 근거

ORD 기록
ord-9f05c8bc582f407aac046856dc43d729
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05225406

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