2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 2,7-Dibromophenanthrene

HRID 751744

반응식

HRID 751744 반응식
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([Br:16])=[CH:10][CH:11]=3)[CH2:6][CH2:5][C:4]=2[CH:3]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C1C=CC=CC=1>[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([Br:16])=[CH:10][CH:11]=3)[CH:6]=[CH:5][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 28250532,7-Dibromo-9,10-dihydrophenanthrene

생성물 1

HCID 111750732,7-Dibromophenanthrene수율 47.7%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Preparing 32.7 g of 2,7-dibromo-9,10-dihydrophenanthrene, 24.1 g of 2,3-dichloro-5,6-dicyanobenzoquinone (DDQ) and 500 milliliter of benzene as a mixture solution, the solution was refluxed with heating under an ambient atmosphere of argon gas for 64 hours. The reacted solution was cooled down to a room temperature, and further filtered. Concentrating the filtrate by means of an evaporator, the residue was washed with a use of methanol. After refining the filtered product by means of a short column, the refined product was re-crystallized with a use of toluene and as a result, 15.5 g of 2,7-dibromophenanthrene was obtained as colorless needle crystals.

후처리

  1. temperaturethe solution was refluxed
  2. temperaturewith heating under an ambient atmosphere of argon gas for 64 hours
  3. concentrationConcentrating the filtrate
  4. customby means of an evaporator
  5. washthe residue was washed with a use of methanol
  6. customthe refined product was re-crystallized with a use of toluene and as a result

출처 및 근거

ORD 기록
ord-56df3de2a9824db3b0fe2b1e3dc6b3ed
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405326B2

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