4-Methoxybenzophenone → 1,1'-[1,2-Bis(4-methoxyphenyl)ethene-1,2-diyl]dibenzene

HRID 924533

반응식

HRID 924533 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1>C1COCC1.[Zn]>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:9]([C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[CH:5][CH:4]=1

참가 물질

4

반응물 1

HCID 691464-Methoxybenzophenone

생성물 1

HCID 665911621,1'-[1,2-Bis(4-methoxyphenyl)ethene-1,2-diyl]dibenzene수율 91%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 8028Tetrahydrofuran용매

실험 절차

A suspension of p-methoxybenzophenone (1.06 g, 5.0 mmol), 1.34 equiv of TiCl3/AlCl3 (5.81 g, 6.7 mmol), and 25 equiv of Zn dust (8.01 g, 122.0 mmol) in 100 ml of dry THF was refluxed for 20 h. The reaction mixture was cooled to room temperature and filtered. The filtrates were evaporated and the crude product was purified by a silica gel column using hexane as eluent. 1,2-Bis(4-methoxyphenyl)-1,2diphenylethene (TPE-OMe) was isolated in 91% yield.

후처리

  1. temperaturewas refluxed for 20 h
  2. filtrationfiltered
  3. customThe filtrates were evaporated
  4. customthe crude product was purified by a silica gel column

출처 및 근거

ORD 기록
ord-662b9fadbf904ee0a0e52dc833a62cbb
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09279806B2

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