Potassium Carbonate → 1,3-bis(4-methoxyphenyl)benzene

HRID 1943534ノート

反応式

HRID 1943534 の反応式
I[C:2]1[CH:7]=[CH:6][CH:5]=[C:4](I)[CH:3]=1.[C:9](=[O:12])([O-])[O-].[K+].[K+]>[Pd].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1.C(O)C.O>[CH3:9][O:12][C:2]1[CH:7]=[CH:6][C:5]([C:2]2[CH:7]=[CH:6][CH:5]=[C:4]([C:2]3[CH:7]=[CH:6][C:5]([O:12][CH3:9])=[CH:4][CH:3]=3)[CH:3]=2)=[CH:4][CH:3]=1

参加物

6

反応物 2

HCID 11430Potassium CarbonateHCID 12270Benzene, 1,3-diiodo-

生成物 1

HCID 46087621,3-bis(4-methoxyphenyl)benzene収率 277.3%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 74236Tetrabutylammonium Bromide触媒HCID 86587398Ethanol toluene water溶媒

実験手順

A mixture of a mixed solvent (toluene/ethanol/water=5/5/1; 1,600 ml), the compound (T-6) (75.9 g, 499.4 mmol), 1,3-diiodobenzene (75.0 g, 227.3 mmol), 5% palladium on carbon (3.75 g), potassium carbonate (94.1 g, 681.0 mmol) and tetrabutylammonium bromide (18.29 g, 56.7 mmol) was refluxed with stirring for 15 hours under an atmosphere of nitrogen. The resulting reaction mixture was cooled to room temperature, and deposits were collected by filtration. The deposits were recrystallized from a mixed solvent of THF and ethyl acetate to give colorless crystals (61.0 g) of 4,4″-dimethoxy-(1,1′:3′,1″)-terphenyl (T-7).

後処理

  1. customThe resulting reaction mixture
  2. filtrationdeposits were collected by filtration
  3. customThe deposits were recrystallized from a mixed solvent of THF and ethyl acetate

出典と根拠

ORDレコード
ord-fad97c459cec4d00824ff02242866704
出典データセット
uspto-grants-2013_03
特許番号
US08394468B2

反応ノート

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