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Toluene → 2-(4-(1,2,2-Triphenylvinyl)phenyl)triphenylene

HRID 871817
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HRID 871817 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:25]=[CH:24][C:23]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[C:16]4[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=4)[C:10]=3[CH:9]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[C:32]1([CH3:38])[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:32]1([C:38]([C:2]2[CH:7]=[CH:6][C:5]([C:8]3[CH:25]=[CH:24][C:23]4[C:22]5[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=5)[C:16]5[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=5)[C:10]=4[CH:9]=3)=[CH:4][CH:3]=2)=[C:38]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 581748542-(4-Bromophenyl)triphenylene

생성물 1

HCID 866753932-(4-(1,2,2-Triphenylvinyl)phenyl)triphenylene수율 82%

시약·촉매·용매 1

HCID 178418397HCID 178418397, 화합물촉매

반응 조건

온도
60 °C

실험 절차

The product B (1.25 g, 3.26 mmol), D (1.37 g, 3.58 mmol), potassium carbonate solution (K2CO3(aq), 2.0 M, 8.0 mL), and dried toluene (24 mL) were charged in a two-necked bottle. The bottle was deoxygenated and purged with nitrogen, and the mixture in the bottle was stirred at 60° C. until it was totally dissolved. The nitrogen pressure of the bottle was increased, and Pd(PPh3)4 (381 mg, 0.33 mmol) was rapidly added into the bottle. The reaction was heated to 110° C., and stirred for 48 hours. The resulting was filtered to remove metal. The filtrate was condensed to remove the solvent. The solid was washed by water and methanol, and then sublimated at a temperature of 260° C. to obtain TSTP (1.50 g, yield=82%) as white solid.

후처리

  1. customThe bottle was deoxygenated
  2. custompurged with nitrogen
  3. dissolutionwas totally dissolved
  4. temperatureThe nitrogen pressure of the bottle was increased
  5. temperatureThe reaction was heated to 110° C.
  6. stirringstirred for 48 hours
  7. filtrationThe resulting was filtered
  8. customto remove metal
  9. customcondensed
  10. customto remove the solvent
  11. washThe solid was washed by water and methanol
  12. customsublimated at a temperature of 260° C.
  13. customto obtain TSTP (1.50 g, yield=82%) as white solid

출처 및 근거

ORD 기록
ord-60257c80087f4d65a7c01d2e724828b9
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08974920B2

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