Isobutylamine → HCID 21512169, Verbindung

HRID 1576347Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1576347
[CH:1]([NH:4][C:5]1[C:18]2[C:17](=[O:19])[C:16]3[C:11](=[C:12]([OH:20])[CH:13]=[CH:14][CH:15]=3)[C:10](=[O:21])[C:9]=2[C:8](Br)=[CH:7][CH:6]=1)([CH3:3])[CH3:2].[CH2:23]([NH2:27])[CH:24]([CH3:26])[CH3:25]>CO.[Cu]Cl.S([O-])([O-])(=O)=O.[Cu+2]>[CH:1]([NH:4][C:5]1[C:18]2[C:17](=[O:19])[C:16]3[C:11](=[C:12]([OH:20])[CH:13]=[CH:14][CH:15]=3)[C:10](=[O:21])[C:9]=2[C:8]([NH:27][CH2:23][CH:24]([CH3:26])[CH3:25])=[CH:7][CH:6]=1)([CH3:3])[CH3:2]

Komponenten

6

Edukt 2

HCID 6558IsobutylamineHCID 215121524-Bromo-5-hydroxy-1-[(1-methylethyl)amino]-9,10-anthracenedione

Produkt 1

HCID 21512169HCID 21512169, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24462Copper SulfateKatalysatorHCID 62652Cuprous chlorideKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

10 Parts 1-isopropylamino-4-bromo-5-hydroxy-anthraquinone, 50 parts isobutylamine, 0.1 part each of copper(I) chloride and basic copper sulphate are boiled under reflux (appr. 70°) until only small amounts of starting material can be detected (appr. 2 hours are required). The mixture is diluted with 50 parts methanol, the precipitated needles are filtered off with suction in the cold, washed with methanol and hot water. It is also possible to filter off with suction without previous dilution with methanol. The 1-isopropylamino-5-hydroxy-4-isobutylamino-anthraquinone so obtained is sulphonated as follows:

Aufarbeitung

  1. temperatureunder reflux (appr. 70°) until only small amounts of starting material
  2. custom(appr. 2 hours are required)
  3. filtrationthe precipitated needles are filtered off with suction in the cold
  4. washwashed with methanol and hot water
  5. filtrationto filter off with suction without previous dilution with methanol

Quellen und Nachweise

ORD-Eintrag
ord-ca7141dec83d42a4928ee4c65c50480e
Quelldatensatz
uspto-grants-1976_09
Patentnummer
US03980677

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