Ammonium Hydroxide → gadolinium(3+);(Z)-4-oxopent-2-en-2-olate

HRID 2361526Notes

Reaction equation

HRID 2361526 reaction equation
[C:1]([CH2:4][C:5](=[O:7])[CH3:6])(=[O:3])[CH3:2].[OH-].[NH4+].[CH3:10]/[C:11](/[O-:16])=[CH:12]/[C:13]([CH3:15])=[O:14].[Cl-].[Gd+3:18].[Cl-].[Cl-]>O>[CH3:6]/[C:5](/[O-:7])=[CH:4]/[C:1]([CH3:2])=[O:3].[CH3:10]/[C:11](/[O-:16])=[CH:12]/[C:13]([CH3:15])=[O:14].[CH3:6]/[C:5](/[O-:7])=[CH:4]/[C:1]([CH3:2])=[O:3].[Gd+3:18]

Participants

6

Reactant 4

HCID 14923Ammonium HydroxideHCID 31261Acetylacetone3×HCID 449676Gadolinium(3+);trichlorideHCID 5460482Acetylacetonate2×

Product 1

HCID 14123091gadolinium(3+);(Z)-4-oxopent-2-en-2-olate

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

Gadolinium acetylacetonate (GdAcAc) was prepared using the method as previously described by Nijsen et al. for holmium acetylacetonate [2-3]. Briefly, 166 g of acetylacetone was dissolved in 1 l of distilled water. The pH of the acetylacetone solution was then adjusted to 8.50 by addition of ammonium hydroxide, thereby ionising the acetylacetone to acetylacetonate. 10 g of gadolinium chloride was dissolved in 40 ml of distilled water and added to the acetylacetonate solution, followed by gentle stirring. The solution was then left to stand overnight at room temperature. The crystals were collected by centrifugation (2 000 rpm for 2 min), washed 4 times with distilled water and dried in two steps: first overnight at room temperature, then overnight at 50° C.

Workup

  1. waitThe solution was then left
  2. customThe crystals were collected by centrifugation (2 000 rpm for 2 min)
  3. washwashed 4 times with distilled water
  4. customdried in two steps
  5. customovernight
  6. customat room temperature
  7. customovernight
  8. customat 50° C.

Sources & evidence

ORD record
ord-fe3c8b9ff26f423a92418fd17387dd15
Source dataset
uspto-grants-2014_04
Patent number
US08691280B2

Reaction notes

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