2-Methoxyethanol → Gadolinium (III) isopropoxide

HRID 432531Notes

Reaction equation

HRID 432531 reaction equation
[CH3:1][CH:2]([CH3:4])[O-:3].[Gd+3:5].[CH3:6][CH:7]([CH3:9])[O-:8].[CH3:10][CH:11]([CH3:13])[O-:12].[CH3:14][O:15][CH2:16][CH2:17]O>>[CH3:1][CH:2]([CH3:4])[O-:3].[Gd+3:5].[CH3:6][CH:7]([CH3:9])[O-:8].[CH3:10][CH:11]([CH3:13])[O-:12].[CH3:14][O:15][CH:16]([CH3:17])[O-:3].[Gd+3:5].[CH3:14][O:15][CH:16]([CH3:17])[O-:3].[CH3:14][O:15][CH:16]([CH3:17])[O-:3]

Participants

4

Reactant 2

HCID 80192-MethoxyethanolHCID 15047187Gadolinium (III) isopropoxide

Product 2

HCID 15047187Gadolinium (III) isopropoxideHCID 131723452Gadolinium(3+);tris(1-methoxyethanolate)

Procedure

Gadolinium isopropoxide was synthesized using the method of Brown et al. The Gd2O3 precursor solution was prepared by reacting 4.85 g (15 mmole) of gadolinium isopropoxide with 50 ml of 2-methoxyethanol under an inert atmosphere. After refluxing for approximately 1 hour, two-thirds of the solution (isopropanol and 2-methoxyethanol) was removed by distillation. The flask was allowed to cool, and 20 ml of 2-methoxyethanol was added. The flask was refluxed for 1 hour, and ⅔ of the solution was then removed by distillation. This process of dilution, reflux, and distillation was repeated for a total of three cycles to ensure the complete exchange of the methoxyethoxide ligand for the isopropoxide ligand. It was estimated that this occurs when the boiling point of the solution reaches 124° C. The final concentration of the solution was adjusted to obtain a 0.5 M solution of gadolinium methoxyethoxide in 2-methoxyethanol. A partially hydrolyzed solution suitable for spin coating or dip-coating was prepared by reacting 1 part of a 1.0 molar solution of water in 2-methoxyethanol with 4 parts of the 0.5 M gadolinium methoxyethoxide solution.

Workup

  1. customwas prepared
  2. temperatureAfter refluxing for approximately 1 hour
  3. customtwo-thirds of the solution (isopropanol and 2-methoxyethanol) was removed by distillation
  4. temperatureto cool
  5. addition20 ml of 2-methoxyethanol was added
  6. temperatureThe flask was refluxed for 1 hour
  7. custom⅔ of the solution was then removed by distillation
  8. temperatureThis process of dilution, reflux
  9. distillationdistillation
  10. customreaches 124° C

Sources & evidence

ORD record
ord-083b20246ecb4ac8b5b7ad55dfaef482
Source dataset
uspto-grants-2003_12
Patent number
US06663976B2

Reaction notes

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