2-Methoxyethanol → Ytterbium(III) isopropoxide

HRID 432532Notes

Reaction equation

HRID 432532 reaction equation
[CH3:1][CH:2]([CH3:4])[O-:3].[Yb+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].[Yb+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].[Yb+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 11198891Ytterbium(III) isopropoxide

Product 2

HCID 11198891Ytterbium(III) isopropoxideHCID 131723453HCID 131723453, compound

Procedure

Ytterbium isopropoxide was synthesized using the method of Brown et al. A flask containing 4.85 g (15 mmole) of ytterbium isopropoxide was reacted 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 ytterbium methoxyethoxide in 2-methoxyethanol. Coating solutions were prepared by reacting 1 part of a 1.0 molar solution of water in 2-methoxyethanol with 4 parts of the 0.5 M ytterbium methoxyethoxide solution.

Workup

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

Sources & evidence

ORD record
ord-d78f781dca2f48e1a4adcd9b77987322
Source dataset
uspto-grants-2003_12
Patent number
US06663976B2

Reaction notes

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