1-Chloroanthraquinone → 1-(1-Ethylpropylamino)anthraquinone

HRID 1376307

反応式

HRID 1376307 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]([CH:20]([NH2:23])[CH2:21][CH3:22])[CH3:19].C([O-])(=O)C.[K+]>[Cu].O>[CH2:18]([CH:20]([NH:23][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)[CH2:21][CH3:22])[CH3:19]

参加物

6

反応物 3

HCID 67091-ChloroanthraquinoneHCID 120193-PentanamineHCID 517044Potassium Acetate

生成物 1

HCID 229162751-(1-Ethylpropylamino)anthraquinone

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 962Water溶媒

反応条件

温度
180 °C

実験手順

A Parr stainless steel high pressure reactor was charged with 1-chloroanthraquinone (24.3 g), 1-ethylpropylamine (17.5 g), potassium acetate.(14.0 g), activated copper metal (0.7 g), and water (0.05 g). The reaction vessel was sealed and heated to a temperature of 180° C. in an oil bath and maintained at that temperature for 12 hours. The oil bath was removed and the vessel was allowed to return to ambient conditions. The solid was extracted with methylene chloride and the insoluble materials removed by filtration. The solvent was removed and the solid recrystallized from hot methanol. The material was chromatographed on a silica gel column using toluene as the eluent.

後処理

  1. customThe reaction vessel was sealed
  2. temperaturemaintained at that temperature for 12 hours
  3. customThe oil bath was removed
  4. extractionThe solid was extracted with methylene chloride
  5. customthe insoluble materials removed by filtration
  6. customThe solvent was removed
  7. customthe solid recrystallized from hot methanol
  8. customThe material was chromatographed on a silica gel column

出典と根拠

ORDレコード
ord-4b619910aa744d42828a8ffc7b87d55a
出典データセット
uspto-grants-1997_09
特許番号
US05663024

関連ノート

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