Ethyl 2-methylacetoacetate → HCID 131733614, compound

HRID 1751168Notes

Reaction equation

HRID 1751168 reaction equation
[OH-].[Na+].[CH3:3][CH:4]([C:10]([CH3:12])=[O:11])[C:5]([O:7]CC)=[O:6].[N+]([O-])(O)=[O:14].[N+]([O-])([O-])=O.[Cu+2:21].[N+]([O-])([O-])=O>>[OH2:6].[OH2:14].[CH3:3][CH:4]([C:10]([CH3:12])=[O:11])[C:5]([O-:7])=[O:6].[Cu+2:21].[CH3:3][CH:4]([C:10]([CH3:12])=[O:11])[C:5]([O-:7])=[O:6]

Participants

5

Reactant 4

HCID 701Ethyl 2-methylacetoacetateHCID 944Nitric AcidHCID 14798Sodium HydroxideHCID 18616Cupric nitrate

Product 1

HCID 131733614HCID 131733614, compound

Conditions

Temperature
30 °C

Procedure

Into a NaOH aqueous solution (3.46 g, 24.0 mL) for hydrolysis, 10.4 g (72.0 mmol) of ethyl 2-methylacetoacetate was added, and stirred under heating at 30° C. for 3 hours. After the three hours, the reaction mixture was cooled down to 0° C., and a 5 N HNO3 aqueous solution was added thereto to make the reaction liquid acidic. To the reaction mixture, 4.34 g (7.20 mmol) of copper (II) nitrate aqueous solution was added dropwise, and subjected to magnetic stirring for 3 hours. The precipitated solid was taken out by filtration, and washed with ion-exchanged water and acetone to obtain 2.81 g (8.52 mmol) of copper (II) 2-methylacetoacetate dihydrate in the form of blue solid.

Workup

  1. additionwas added
  2. temperatureAfter the three hours, the reaction mixture was cooled down to 0° C.
  3. customthe reaction liquid acidic
  4. stirringto magnetic stirring for 3 hours
  5. filtrationThe precipitated solid was taken out by filtration
  6. washwashed with ion-exchanged water and acetone

Sources & evidence

ORD record
ord-8ef6dabbe1ec441c9cffc38ba12e107d
Source dataset
uspto-grants-2015_10
Patent number
US09157004B2

Reaction notes

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