1-Chloroanthraquinone → 1-(n-Octylsulfonylamino)anthraquinone

HRID 1087301

反応式

HRID 1087301 の反応式
Cl[C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH2:18]([S:26]([NH2:29])(=[O:28])=[O:27])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C(=O)([O-])[O-].[K+].[K+]>C([O-])(=O)C.[Cu+2].C([O-])(=O)C.ClC1C=CC=CC=1Cl>[CH2:18]([S:26]([NH:29][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1)(=[O:27])=[O:28])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

参加物

6

反応物 3

HCID 67091-ChloroanthraquinoneHCID 11430Potassium CarbonateHCID 2295971-Octanesulfonamide

生成物 1

HCID 199903611-(n-Octylsulfonylamino)anthraquinone

試薬・触媒・溶媒 2

HCID 8895Cupric acetate触媒HCID 72391,2-Dichlorobenzene溶媒

実験手順

A 100ml round bottom flask, equipped with a magnetic stirrer and cooling condenser, was charged with 1-chloroanthraquinone (2.0g), n-octylsulfonamide (3.0g), copper acetate (0.8g), potassium carbonate (0.8g) and o-dichlorobenzene (25ml). This mixture was slowly heated to reflux. After 2.5 hours the reaction mixture was cooled and filtered. Methanol was then added to induce precipitation, and after filtration the solid was recrystallized from a mixture of dichloromethane and methanol to give a yellow product.

後処理

  1. customA 100ml round bottom flask, equipped with a magnetic stirrer
  2. temperaturecooling condenser
  3. temperatureThis mixture was slowly heated to reflux
  4. temperatureAfter 2.5 hours the reaction mixture was cooled
  5. filtrationfiltered
  6. additionMethanol was then added
  7. customprecipitation
  8. filtrationafter filtration the solid
  9. customwas recrystallized from a mixture of dichloromethane and methanol
  10. customto give a yellow product

出典と根拠

ORDレコード
ord-3e6a13242a364f83931fe3aa4a4de4e3
出典データセット
uspto-grants-1991_07
特許番号
US05034547

関連ノート

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