1,3-Diphenylisobenzofuran → 3-Bromo-7,12-diphenylbenzo[k]fluoranthene

HRID 1012678노트

반응식

HRID 1012678 반응식
[Br:1][C:2]1[C:12]2[C:13]3[C:5]([CH:6]=[CH:7][C:8]=3[CH:9]=[CH:10][CH:11]=2)=[CH:4][CH:3]=1.[C:14]1([C:20]2O[C:22]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[C:23]3[C:28]=2[CH:27]=[CH:26][CH:25]=[CH:24]3)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C1(C)C(C)=CC=CC=1>[Br:1][C:2]1[C:12]2[C:13]3[C:5]([C:6]4[C:20]([C:14]5[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=5)=[C:28]5[CH:27]=[CH:26][CH:25]=[CH:24][C:23]5=[C:22]([C:29]5[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=5)[C:7]=4[C:8]=3[CH:9]=[CH:10][CH:11]=2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 216491,3-DiphenylisobenzofuranHCID 122444035-Bromoacenaphthylene

생성물 1

HCID 107909823-Bromo-7,12-diphenylbenzo[k]fluoranthene수율 52.7%

시약·촉매·용매 1

HCID 7237O-Xylene용매2회

실험 절차

200 ml of xylene was added to a mixture of 5-bromoacenaphthylene (14.5 g, 62.8 mmol) and diphenylisobenzofuran (17.1 g, 63.3 mmol), and stirred for 5 hours under reflux of xylene. The mixture obtained was cooled to room temperature, and thereafter the solvent was distilled off, and 26 ml of trifluoroacetic anhydride and 260 ml of chloroform were added thereto and stirred for 1 hour under reflux. The mixture obtained was cooled to room temperature, and thereafter the solvent was distilled off, and then the resultant residue was purified by silica gel column chromatography (mobile phase; toluene:heptane=1:3) to produce as a yellow solid 16 g of 4-bromo-7,12-diphenylbenzo[k]fluoranthene.

후처리

  1. customThe mixture obtained
  2. distillationthe solvent was distilled off
  3. addition26 ml of trifluoroacetic anhydride and 260 ml of chloroform were added
  4. stirringstirred for 1 hour
  5. temperatureunder reflux
  6. customThe mixture obtained
  7. temperaturewas cooled to room temperature
  8. distillationthe solvent was distilled off
  9. customthe resultant residue was purified by silica gel column chromatography (mobile phase; toluene:heptane=1:3)

출처 및 근거

ORD 기록
ord-03e769965f464c9e86ad36e1eae50bea
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977869B2

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