2-Methoxyethanol → Gadolinium (III) isopropoxide

Participants

Reaction Steps

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.

Provenance & Evidence