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

HRID 260815

反応式

HRID 260815 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 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. customThe oil bath was removed
  3. extractionThe solid was extracted with methylene chloride
  4. customthe insoluble materials removed by filtration
  5. customThe solvent was removed
  6. customthe solid recrystallized from hot methanol
  7. customThe material was chromatographed on a silica gel column

出典と根拠

ORDレコード
ord-6cfbd3d55d5b49c084c94cd2254a7046
出典データセット
uspto-grants-1996_06
特許番号
US05530053

関連ノート

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