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

HRID 2079445
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HRID 2079445 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7243O-PhenylenediamineHCID 964304,4'-Dibromobenzil

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
80 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-d5be39fa67fd4c1ab732e22a2e8b70ad
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07931974B2

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