Acetylacetone → HCID 159868, compound

HRID 843381Notes

Reaction equation

HRID 843381 reaction equation
[OH-].[Ca+2:2].[OH-].[C:4]([CH2:7][C:8](=[O:10])[CH3:9])(=[O:6])[CH3:5]>>[CH3:9][C:8]([O-:10])=[CH:7][C:4]([CH3:5])=[O:6].[CH3:9][C:8]([O-:10])=[CH:7][C:4]([CH3:5])=[O:6].[Ca+2:2]

Participants

3

Reactant 2

HCID 31261AcetylacetoneHCID 6093208Calcium Hydroxide

Product 1

HCID 159868HCID 159868, compoundYield 99.7%

Procedure

444 g (6 mol) of calcium hydroxide was added to the kneader used in Comparative Example 1, and stirred. Thereafter, 1,320 g [13.2 mol, calcium hydroxide/acetylacetone=1/2.2 (molar ratio)] of acetylaceton was dropped into the kneader over 3 hours. The reaction temperature was between 43 and 65° C. After completion of the dropping, at a temperature of from 65 to 66° C., the mixture was stirred and mixed for aging over 4 hours until the reaction was complete. The resultant powder was slightly moisture-laden. The resulting product was warmed under a flow of nitrogen gas. At the point where the temperature reached 68° C., the product was subjected to the drying step, and dried at 106 to 138° C. for 10 hours until the moisture or water content was reduced to 0.46% by weight. Thereafter, the dried product was cooled to give 1,425 g of white calcium acetylacetonate [yield 98.2 mol % (calcium hydroxide basis), purity 98.6% by weight].

Workup

  1. customwas between 43 and 65° C
  2. stirringAfter completion of the dropping, at a temperature of from 65 to 66° C., the mixture was stirred
  3. additionmixed
  4. temperatureThe resulting product was warmed under a flow of nitrogen gas
  5. customreached 68° C.
  6. dry with materialdried at 106 to 138° C. for 10 hours until the moisture or water content
  7. temperatureThereafter, the dried product was cooled

Sources & evidence

ORD record
ord-a2ace98691444de78510c1343c88d34b
Source dataset
uspto-grants-2002_04
Patent number
US06376719B1

Reaction notes

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