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

HRID 414753
ノート
印刷プレビュー

反応式

HRID 414753 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

反応条件

温度
-60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3662bedfbbfa4b4dadd802fd3f06f835
出典データセット
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04794155

反応ノート

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