Sulfuric Acid → HCID 178507708, Verbindung

HRID 1262493Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1262493
[NH2:1][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[C:5]([NH2:18])=[CH:4][CH:3]=1.[NH2:19][C:20]1[C:33]2[C:32](=[O:34])[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:25](=[O:35])[C:24]=2[CH:23]=[CH:22][CH:21]=1.OS(O)(=O)=O.[K]>O>[CH:10]1[CH:9]=[C:8]2[C:7]([C:6]3[C:15]([C:14](=[O:16])[C:13]2=[CH:12][CH:11]=1)=[C:2]([NH:1][C:23]1[CH:22]=[CH:21][C:20]([NH2:19])=[C:33]2[C:32]([C:31]4[C:26]([C:25](=[O:35])[C:24]=12)=[CH:27][CH:28]=[CH:29][CH:30]=4)=[O:34])[CH:3]=[CH:4][C:5]=3[NH2:18])=[O:17]

Komponenten

6

Edukt 4

HCID 1118Sulfuric AcidHCID 67101-AminoanthraquinoneHCID 31420Disperse Violet 1HCID 5462222Potassium

Produkt 1

HCID 178507708HCID 178507708, VerbindungAusbeute 99,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 52.0 g of 1,4-diaminoanthraquinone (92% pure) and 47.0 g of 1-aminoanthraquinone (98% pure) in 410 g of 96% strength H2SO4 is added dropwise to 410 g of water. 95.0 g of potassium peroxodisulphate is introduced into the red-orange paste at 40°-50° C. within 1 hour, the mixture is stirred for approximately a further 30 minutes and the solid is filtered off with suction. The filter cake is washed to neutrality and then stirred briefly in a mixture of 100 ml of 40% strength NaHSO3 solution and 400 ml of water. The solid is then filtered off with suction, washed with water and dried at 100° C. 96.5 g of 4,4'-diamino-1,1'-dianthrimide (84% pure), corresponding to 88% of theory, are isolated.

Aufarbeitung

  1. filtrationthe solid is filtered off with suction
  2. washThe filter cake is washed to neutrality
  3. stirringstirred briefly in a mixture of 100 ml of 40% strength NaHSO3 solution and 400 ml of water
  4. filtrationThe solid is then filtered off with suction
  5. washwashed with water
  6. customdried at 100° C

Quellen und Nachweise

ORD-Eintrag
ord-f5a05c2c42014556885ed2e0728e1898
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04452742

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