反应 #2819209
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06663976B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. After refluxing for approximately 1 hour two-thirds of the solution (isopropanol and 2-methoxyethanol) was removed by distillation to cool 20 ml of 2-methoxyethanol was added The flask was refluxed for 1 hour ⅔ of the solution was then removed by distillation This process of dilution, reflux distillation reaches 124° C
来源 ID: ord-d78f781dca2f48e1a4adcd9b77987322