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

HRID 1943534노트

반응식

HRID 1943534 반응식
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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 74236Tetrabutylammonium Bromide촉매HCID 86587398Ethanol toluene water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fad97c459cec4d00824ff02242866704
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394468B2

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