Phenol → 1,8-Diphenoxyanthraquinone

HRID 127167

反応式

HRID 127167 の反応式
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-:8].[K+].Cl[C:11]1[C:24]2[C:23](=[O:25])[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][C:21]=3[N+]([O-])=O)[C:16](=[O:29])[C:15]=2[CH:14]=[CH:13][CH:12]=1>>[O:7]([C:11]1[C:24]2[C:23](=[O:25])[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][C:21]=3[O:8][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:16](=[O:29])[C:15]=2[CH:14]=[CH:13][CH:12]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 3

HCID 996PhenolHCID 14797Potassium HydroxideHCID 2257041-Nitro-8-chloroanthraquinone

生成物 1

HCID 665011,8-Diphenoxyanthraquinone

反応条件

温度
100 °C

実験手順

A mixture of 21 g. phenol, 13 g. potassium hydroxide and 270 g. o-chlorotoluene was converted to a water-free slurry of potassium phenoxide by azeotropic distillation of all the water formed. After cooling back to 100° C., 28.8 g. of 1-chloro-8-nitroanthraquinone was charged and the whole heated and stirred at 130° C. for 6 hours. The product was isolated by steam distillation, filtration, washing and drying. A 37.7 g. yield (96.2% of theory) of a product identical to authentic 1,8-diphenoxyanthraquinone in a thin layer chromatogram and free of starting material was obtained.

後処理

  1. additionA mixture of 21 g
  2. distillationo-chlorotoluene was converted to a water-free slurry of potassium phenoxide by azeotropic distillation of all the water
  3. customformed
  4. temperaturethe whole heated
  5. customThe product was isolated by steam distillation, filtration
  6. washwashing
  7. customdrying

出典と根拠

ORDレコード
ord-a1f80f2135794476b69ab2f82b7dcaa3
出典データセット
uspto-grants-1981_03
特許番号
US04255342

関連ノート

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