P-Anisidine → 1-p-Anisidino-8-nitro-anthraquinone

HRID 1729570

반응식

HRID 1729570 반응식
[N+:1]([C:4]1[C:17]2[C:16](=[O:18])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][C:14]=3[N+:19]([O-:21])=[O:20])[C:9](=[O:22])[C:8]=2[CH:7]=[CH:6][CH:5]=1)([O-])=O.[CH3:23][O:24][C:25]1[CH:30]=[CH:29][C:28](N)=[CH:27][CH:26]=1.C([O-])(=O)C.[K+]>CO>[CH3:23][O:24][C:25]1[CH:30]=[CH:29][C:28]([NH:1][C:4]2[C:17]3[C:16](=[O:18])[C:15]4[C:10](=[CH:11][CH:12]=[CH:13][C:14]=4[N+:19]([O-:21])=[O:20])[C:9](=[O:22])[C:8]=3[CH:7]=[CH:6][CH:5]=2)=[CH:27][CH:26]=1

참가 물질

5

반응물 3

HCID 7732P-AnisidineHCID 672101,8-Dinitro-9,10-anthraquinoneHCID 517044Potassium Acetate

생성물 1

HCID 203164861-p-Anisidino-8-nitro-anthraquinone수율 81.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 50 g of 1,8-dinitro-anthraquinone (82% strength), 150 g of p-anisidine and 21.5 g of anhydrous potassium acetate is heated at 95° - 100° C (duration approx. 5 hours), with vigorous stirring, until no further starting material is present, according to thin layer chromatography. The mixture is diluted with 150 ml of methanol over the course of 30 minutes at 50° - 60° C and is stirred overnight until cold and the reaction product is filtered off, washed with a solution of 30 g of p-anisidine in 30 ml of methanol and finally with 200 ml of methanol and hot water, and dried at 80° C. 51 g of 1-p-anisidino-8-nitro-anthraquinone are obtained.

후처리

  1. temperatureis heated at 95° - 100° C (duration approx. 5 hours)
  2. filtrationis filtered off
  3. washwashed with a solution of 30 g of p-anisidine in 30 ml of methanol and finally with 200 ml of methanol and hot water
  4. customdried at 80° C

출처 및 근거

ORD 기록
ord-0bba9ba4652b4da69abc6bf80b5393bb
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03989450

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