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Potassium Carbonate → (E)-2-(4-Styrylphenyl)triphenylene

HRID 871816
ノート
印刷プレビュー

反応式

HRID 871816 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.[CH:26](/B(O)O)=[CH:27]\[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(=O)([O-])[O-].[K+].[K+]>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.C1(C)C=CC=CC=1>[CH:26](/[C:2]1[CH:3]=[CH:4][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:6][CH:7]=1)=[CH:27]\[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=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

6

反応物 3

HCID 11430Potassium CarbonateHCID 5702628Styrylboronic acidHCID 581748542-(4-Bromophenyl)triphenylene

生成物 1

HCID 86675392(E)-2-(4-Styrylphenyl)triphenylene収率 75%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 1140
Toluene
溶媒

反応条件

温度
60 °C

実験手順

The product B (400 mg, 1.04 mmol) or B1, (E)-styrylboronic acid (185 mg, 1.25 mmol), potassium carbonate solution (2.0 M, 4.0 mL) and dried toluene (12 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 (120 mg, 0.1 mmol) was rapidly added into the bottle. The reaction was heated to 110° C., and stirred for 48 hours. The resulting was cooled to room temperature to precipitate a solid, and the solid was collected by filtering. The solid was washed by water and methanol, and then sublimated at a temperature of 230° C. to obtain TSP (317 mg, yield=75%) 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. temperatureThe resulting was cooled to room temperature
  8. customto precipitate a solid
  9. customthe solid was collected
  10. filtrationby filtering
  11. washThe solid was washed by water and methanol
  12. customsublimated at a temperature of 230° C.
  13. customto obtain TSP (317 mg, yield=75%) as white solid

出典と根拠

ORDレコード
ord-30ee0fc6fcad48279e8e5d32e6e8dd03
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