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Hydrochloric Acid → Methanone, 1,3-phenylenebis[(4-phenoxyphenyl)-

HRID 414753
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인쇄 미리보기

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HRID 414753 반응식
[C:1]1([O:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Cl-].[Cl-].[Al+3].[C:18](Cl)(=[O:28])[C:19]1[CH:27]=[CH:26][CH:25]=[C:21]([C:22](Cl)=[O:23])[CH:20]=1.Cl>ClCCl>[O:7]([C:1]1[CH:2]=[CH:3][C:4]([C:18]([C:19]2[CH:27]=[CH:26][CH:25]=[C:21]([C:22](=[O:23])[C:11]3[CH:12]=[CH:13][C:8]([O:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)=[CH:9][CH:10]=3)[CH:20]=2)=[O:28])=[CH:5][CH:6]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7451Isophthaloyl chlorideHCID 7583Diphenyl EtherHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 11070706Methanone, 1,3-phenylenebis[(4-phenoxyphenyl)-수율 61%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

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온도
-60 °C

실험 절차

Diphenyl oxide (51 g), 100 ml of dichloromethane and 13.3 g of aluminum trichloride are placed in a flask equipped with a mechanical stirrer, a reflux condenser and an addition funnel. After cooling the flask to -60° C., 10.15 g of isophthaloyl chloride is added over a 30-minute period. The reaction is stirred at 25° C. for 72 hours and refluxed for 4 hours. The reaction mixture is poured into 100 ml of 1M hydrochloric acid and the organic layer is washed once with ammonium hydroxide and twice with water. The organic layer is dried with sodium bisulfate and the solvent is evaporated. The product is recrystallized from methylethyl ketone, yielding 14.3 g (61 percent yield) of the title compound.

후처리

  1. customequipped with a mechanical stirrer, a reflux condenser and an addition funnel
  2. temperaturerefluxed for 4 hours
  3. washthe organic layer is washed once with ammonium hydroxide and twice with water
  4. dry with materialThe organic layer is dried with sodium bisulfate
  5. customthe solvent is evaporated
  6. customThe product is recrystallized from methylethyl ketone

출처 및 근거

ORD 기록
ord-3662bedfbbfa4b4dadd802fd3f06f835
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04794155

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