Hydrogen Bromide → 4,5-Dinitrobenzene-1,2-diol

HRID 346401노트

반응식

HRID 346401 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.Br>O>[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 260Hydrogen BromideHCID 2229891,2-Dimethoxy-4,5-dinitrobenzene

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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

후처리

  1. temperatureunder refluxing for 6 hours
  2. extractionThe solution was extracted three times with ethyl acetate
  3. washThe organic layer was washed with a 10% sodium hydrogencarbonate
  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-882ae4136e174d48a2245dc5dedf0898
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05061794

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