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Sodium Carbonate → HCID 23080768、化合物

HRID 2274134
ノート
印刷プレビュー

反応式

HRID 2274134 の反応式
[CH:1]1[C:15]2=[C:16]3[C:8]([C:9]4[C:14]2=[CH:13][CH:12]=[CH:11][CH:10]=4)=[CH:7][CH:6]=[CH:5][C:4]3=[C:3](B(O)O)[CH:2]=1.[Br:20][C:21]1[CH:26]=[CH:25][C:24](I)=[CH:23][CH:22]=1.C(=O)([O-])[O-].[Na+].[Na+]>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>[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:5]2[CH:6]=[CH:7][C:8]3[C:9]4[C:14]([C:15]5[C:16]=3[C:4]=2[CH:3]=[CH:2][CH:1]=5)=[CH:13][CH:12]=[CH:11][CH:10]=4)=[CH:23][CH:22]=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 10340Sodium CarbonateHCID 115221-Bromo-4-iodobenzeneHCID 23088535Fluoranthen-3-ylboronic acid

生成物 1

HCID 23080768HCID 23080768、化合物収率 70%

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
100 °C

実験手順

In the atmosphere of argon, 9.1 g of fluoranthene-3-boronic acid, 10.5 g of 4-bromoiodobenzene, 2.1 g of tetrakis(triphenylphosphine)palladium(0), 186 mL of toluene and 74 mL of an aqueous 2M solution of sodium carbonate were placed in a flask, and stirred at 100° C. for 8 hours. After cooling to room temperature, the reaction solution was extracted with toluene. After removing an aqueous phase, an organic phase was washed with saturated saline, and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure, and residues were purified by silica gel column chromatography, whereby 9.2 g (yield 70%) of 3-(4-bromophenyl)fluoranthene as an intended product was obtained.

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionthe reaction solution was extracted with toluene
  3. customAfter removing an aqueous phase
  4. washan organic phase was washed with saturated saline
  5. dry with materialdried with anhydrous sodium sulfate
  6. filtrationAfter filtration
  7. distillationthe solvent was distilled off under reduced pressure, and residues

出典と根拠

ORDレコード
ord-6e48f012d5db44eb8ee79e18550e4d18
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09126943B2

反応ノート

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