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Toluene → HCID 59524089、化合物

HRID 1431036
ノート
印刷プレビュー

反応式

HRID 1431036 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:22]=[C:23](I)[CH:24]=[CH:25][CH:26]=1.C1(C)C=CC=CC=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.CO.O.C(COC)OC>[Br:20][C:21]1[CH:22]=[C:23]([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:24]=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 11561Benzene, 1-bromo-3-iodo-HCID 23088535Fluoranthen-3-ylboronic acid

生成物 1

HCID 59524089HCID 59524089、化合物収率 70.4%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

18.18 g (81.3 mmol) of 3-fluorantheneboronic acid, 22.99 g (81.3 mmol) of 3-bromoiodobenzene, 4.70 g (4.10 mmol) of tetrakis(triphenylphosphine)palladium (0), 80 ml of toluene, 80 ml of dimethoxyethane and 123 g of a 2M sodium carbonate aqueous solution were combined under argon atmosphere, and the mixture was stirred for 8 hours with refluxing and heating. After finishing the reaction, water was added to the reaction mixture, and the mixture was stirred at room temperature for one hour. Methanol was added thereto, and a solid matter was obtained by filtering, and it was refined by silica gel chromatography to obtain 20.43 g (yield: 70.4%) of 3-(3-bromophenyl)fluoranthene.

後処理

  1. temperaturewith refluxing
  2. temperatureheating
  3. additionwas added to the reaction mixture
  4. stirringthe mixture was stirred at room temperature for one hour
  5. customa solid matter was obtained
  6. filtrationby filtering

出典と根拠

ORDレコード
ord-016d8bebb6aa43278f73be733fc216d2
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08941099B2

反応ノート

読み込み中…

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