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

HRID 2418996

Reaktionsgleichung

Reaktionsgleichung von HRID 2418996
[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

Komponenten

5

Edukt 3

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

Produkt 1

HCID 203164861-p-Anisidino-8-nitro-anthraquinone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. additionA mixture of 50 g
  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

Quellen und Nachweise

ORD-Eintrag
ord-70d7d2e2fed24dc581be857afa5daee4
Quelldatensatz
uspto-grants-1978_08
Patentnummer
US04104284

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