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O-Phenylenediamine → 2,3-Bis(4-bromophenyl)quinoxaline

HRID 888702
ノート
印刷プレビュー

反応式

HRID 888702 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][CH:13]=2)=O)=O)=[CH:4][CH:3]=1.[C:19]1([NH2:26])[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[NH2:25]>C(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:10]([C:12]3[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][CH:13]=3)=[N:26][C:19]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[N:25]=2)=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7243O-PhenylenediamineHCID 964304,4'-Dibromobenzil

生成物 1

HCID 5549772,3-Bis(4-bromophenyl)quinoxaline収率 99%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
80 °C

実験手順

30.2 g of 4,4′-dibromobenzil (82.0 mmol), 9.31 g of 1,2-phenylenediamine (86.1 mmol), and 300 mL of chloroform were put into a 500 mL three-necked flask. This reaction solution was refluxed for five hours at 80° C. under a nitrogen gas stream. After the reaction, the reaction solution was cooled to room temperature and washed with water. A water layer was extracted with chloroform, the extracted solution and an organic layer were dried by magnesium sulphate. After drying, the mixture was filtrated by suction to concentrate the filtrate. The obtained solid was dissolved in toluene and this solution was filtrated by suction through Florisil, celite, and alumina. The filtrate was condensed, and 30 g of an objective matter, a white powder solid, 2,3-bis(4-bromophenyl)quinoxaline was obtained at the yield 99%.

後処理

  1. customAfter the reaction
  2. temperaturethe reaction solution was cooled to room temperature
  3. washwashed with water
  4. extractionA water layer was extracted with chloroform
  5. dry with materialthe extracted solution and an organic layer were dried by magnesium sulphate
  6. customAfter drying
  7. filtrationthe mixture was filtrated by suction
  8. concentrationto concentrate the filtrate
  9. dissolutionThe obtained solid was dissolved in toluene
  10. filtrationthis solution was filtrated by suction through Florisil, celite, and alumina
  11. customcondensed, and 30 g of an objective matter

出典と根拠

ORDレコード
ord-02b5a0b701224521acc46da9f429bb1e
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252433B2

反応ノート

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