Ammonia → Cobalt(3+) acetylacetonate

HRID 436286

Reaktionsgleichung

Reaktionsgleichung von HRID 436286
[CH3:1]/[C:2](/[OH:7])=[CH:3]\[C:4]([CH3:6])=[O:5].[CH3:8]/[C:9](/[OH:14])=[CH:10]/[C:11]([CH3:13])=[O:12].[Co].[Co:16](Cl)Cl.[C:19]([CH2:22][C:23](=[O:25])[CH3:24])(=[O:21])[CH3:20].N.OO>CO.O>[CH3:6][C:4]([CH2:3][C:2]([CH3:1])=[O:7])=[O:5].[CH3:13][C:11]([CH2:10][C:9]([CH3:8])=[O:14])=[O:12].[CH3:20][C:19]([CH2:22][C:23]([CH3:24])=[O:25])=[O:21].[Co:16]

Komponenten

8

Edukt 5

HCID 222AmmoniaHCID 784Hydrogen Peroxide2×HCID 24288Cobalt(II) chlorideHCID 31261Acetylacetone2×HCID 5884498Cobalt (II) acetylacetonate

Produkt 1

HCID 407384Cobalt(3+) acetylacetonate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

582.5 grams cobalt(II)acetylacetonate, made from cobalt dichloride and acetylacetone by reaction with ammonia, having a water content of 11.7% by weight, corresponding to 509.6 grams of the anhydrous compound, were dissolved in 2 liters of methanol at room temperature and thereto 210 grams of acetylacetone were added at 35° C, while stirring. Subsequently, to the clear solution 150 grams hydrogen peroxide of about 30% were added within 8 minutes, which led to an increase in temperature of the solution to 65° C. The solution was then stirred at 65° C for about 30 minutes, and another 80 grams of about 30% hydrogen peroxide were added until the solution had turned to a clear green color. Thereafter, the reaction mixture was heated to reflux for one hour, cooled to 3° C, and the precipitated cobalt(III)acetylacetonate filtered and washed with 100 ml of cold methanol. After drying at 5 torr/80° C for 5 hours, 539 grams cobalt(III)acetylacetonate were obtained (corresponding to 75.7% of the theoretical). The product was black and shining, and of finely-crystalline structure, and having a water content of less than 0.05% by weight.

Aufarbeitung

  1. stirringThe solution was then stirred at 65° C for about 30 minutes
  2. temperatureThereafter, the reaction mixture was heated
  3. temperatureto reflux for one hour
  4. temperaturecooled to 3° C
  5. filtrationthe precipitated cobalt(III)acetylacetonate filtered
  6. washwashed with 100 ml of cold methanol
  7. customAfter drying at 5 torr/80° C for 5 hours

Quellen und Nachweise

ORD-Eintrag
ord-c9bfa59fbed14fe2a256e7d4b5e260a2
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04008260

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