p-Toluidine → 9,10-Anthracenedione, 1-(methylamino)-4-[(4-methylphenyl)amino]-

HRID 1199755

反応式

HRID 1199755 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1.[CH3:9][NH:10][C:11]1[C:24]2[C:23](=[O:25])[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16](=[O:26])[C:15]=2[C:14](Br)=[CH:13][CH:12]=1.C([O-])(=O)C.[Na+]>CO.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[CH3:9][NH:10][C:11]1[C:24]2[C:23](=[O:25])[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16](=[O:26])[C:15]=2[C:14]([NH:1][C:2]2[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=2)=[CH:13][CH:12]=1

参加物

6

反応物 3

HCID 7813p-ToluidineHCID 314189,10-Anthracenedione, 1-bromo-4-(methylamino)-HCID 517045Sodium Acetate

生成物 1

HCID 671959,10-Anthracenedione, 1-(methylamino)-4-[(4-methylphenyl)amino]-収率 82%

試薬・触媒・溶媒 2

HCID 8895Cupric acetate触媒HCID 887Methanol溶媒

実験手順

In a reactor were charged p-toluidine (80 parts), 1-methylamino-4-bromoanthraquinone (15.8 parts), sodium acetate (7.5 parts) and copper acetate (0.5 part) and the mixture was kept at 115° to 120° C. for 6 hours under a nitrogen atmosphere. Thereafter, the reaction mixture was diluted with methanol (100 parts) and cooled. The precipitate produced was filtrated, washed with methanol (500 parts) and then water (200 parts), and dried at 80° to 90° C. to obtain 1-methylamino-4-(4'-methylanilino)-anthraquinone (yield 82%).

後処理

  1. temperaturecooled
  2. customThe precipitate produced
  3. filtrationwas filtrated
  4. washwashed with methanol (500 parts)
  5. dry with materialwater (200 parts), and dried at 80° to 90° C.

出典と根拠

ORDレコード
ord-898959b639a845fca73b13ecc9ee2bad
出典データセット
uspto-grants-1990_02
特許番号
US04902798

関連ノート

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