Acetylacetone → HCID 159868, compound
Reaction equation
[C:1]([CH2:4][C:5](=[O:7])[CH3:6])(=[O:3])[CH3:2].[OH-].[Ca+2:9].[OH-]>>[CH3:6][C:5]([O-:7])=[CH:4][C:1]([CH3:2])=[O:3].[CH3:6][C:5]([O-:7])=[CH:4][C:1]([CH3:2])=[O:3].[Ca+2:9]Participants
Procedure
1,202 g (12.0 mol) of acetylacetone was added to a 3 liter kneader equipped with a thermometer, a dropping funnel, a condenser and a jacket, and then stirred. Then 444 g [6 mol, calcium hydroxide/acetylacetone=1/2.0 (molar ratio)] of calcium hydroxide was added dropwise to the kneader over 3 hours. The reaction temperature was between 32 and 65° C. After completion of the dropping, the mixture was stirred and mixed at a temperature of 65 to 68° C. for 4 hours until the reaction was complete. The resulting product was warmed under a flow of nitrogen gas. At 68° C., the product was subjected to the drying step, and dried at 68 to 73° C. for 24 hours until the product attained a moisture content of 6.8% by weight. The dried product was cooled to give 1,550 g of yellowish white calcium acetylacetonate [yield 99.1 mol % (calcium hydroxide basis), purity 91.5% by weight].
Workup
- customkneader equipped with a thermometer, a dropping funnel, a condenser
- customwas between 32 and 65° C
- stirringAfter completion of the dropping, the mixture was stirred
- additionmixed at a temperature of 65 to 68° C. for 4 hours until the reaction
- temperatureThe resulting product was warmed under a flow of nitrogen gas
- customAt 68° C.
- customdried at 68 to 73° C. for 24 hours until the product
- temperatureThe dried product was cooled
Sources & evidence
- ORD record
- ord-ad4d09ffddf04f9e9bf772a27dd0efbe
- Source dataset
- uspto-grants-2002_04
- Patent number
- US06376719B1
Reaction notes
Loading…