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

HRID 751744

反応式

HRID 751744 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 111750732,7-Dibromophenanthrene収率 47.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-56df3de2a9824db3b0fe2b1e3dc6b3ed
出典データセット
uspto-grants-2008_07
特許番号
US07405326B2

関連ノート

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