p-Toluidine → 1-(Methylamino)-4-((4-methylphenyl)amino)anthraquinone

HRID 2380394

반응식

HRID 2380394 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 671951-(Methylamino)-4-((4-methylphenyl)amino)anthraquinone수율 82%

시약·촉매·용매 2

HCID 8895Cupric acetate촉매HCID 887Methanol용매

실험 절차

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% ).

후처리

  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.

출처 및 근거

ORD 기록
ord-afd62127cb4647ccb6659aacef3f72ed
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05367075

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