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

HRID 871817
ノート
印刷プレビュー

反応式

HRID 871817 の反応式
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
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

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 178418397HCID 178418397、化合物触媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-60257c80087f4d65a7c01d2e724828b9
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08974920B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート