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Hydrogen Peroxide → HCID 10989376、化合物

HRID 2257430
ノート
印刷プレビュー

反応式

HRID 2257430 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][C:14](Br)=[CH:13][CH:12]=2)=[CH:5][CH:4]=1)#[N:2].CN1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+].OO>O1CCCC1.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:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][C:14](/[CH:20]=[CH:21]/[CH2:22][CH2:23][CH3:24])=[CH:13][CH:12]=2)=[CH:5][CH:4]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 784Hydrogen PeroxideHCID 11430Potassium CarbonateHCID 12291N-MethylpiperidineHCID 14798Sodium HydroxideHCID 229228794-[(4-Bromophenyl)ethynyl]benzonitrile

生成物 1

HCID 10989376HCID 10989376、化合物収率 84%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

In a four necked flask equipped with a stirrer, a reflux condenser and a thermometer which had been replaced by a nitrogen atmosphere, 1-(4-cyanophenyl)-2-(4-bromophenyl)acetylene (3.4 g, 12 mmol), tetrakis(triphenylphosphine)palladium (0.23 g, 0.2 mmol), N-methylpiperidine (5 g), potassium carbonate (5.5 g, 40 mmol) and tetrahydrofuran (60 ml) were charged. Then, to the mixture, a solution of E-1-pentenylcatecholborane (20 mmol) in tetrahydrofuran (50 ml) was dropwise added at room temperature, followed by heat refluxing for 6 hours while stirring. After cooling the reaction mixture to room temperature, 10% aqueous solution of sodium hydroxide (5 ml) and 30% aqueous hydrogen peroxide (2 ml) were added to the mixture, followed by stirring for 1 hour. The mixture was extracted with ethyl ether. The organic layer was washed with saturated aqueous solution of sodium chloride (20 ml each) twice and dried over anhydrous magnesium sulfate. After evaporating the solvent off, the residue was purified by silica gel column chromatography to obtain 1-(4-cyanophenyl)-2-[4-(1-trans-pentenyl)phenyl]acetylene (2.7 g). Yield: 84%.

後処理

  1. customIn a four necked flask equipped with a stirrer, a reflux condenser
  2. additionwere charged
  3. temperatureby heat
  4. temperaturerefluxing for 6 hours
  5. stirringby stirring for 1 hour
  6. extractionThe mixture was extracted with ethyl ether
  7. washThe organic layer was washed with saturated aqueous solution of sodium chloride (20 ml each) twice
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customAfter evaporating the solvent off, the residue
  10. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-aa6d3758769d4f76899b3b54367f78ec
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05658489

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート