Preparation of cerium halide solvate complexes
View Patent ↗Crystals of a solvated cerium(III) halide solvate complex resulted from a process of forming a paste of a cerium(III) halide in an ionic liquid, adding a solvent to the paste, removing any undissolved solid, and then cooling the liquid phase. Diffusing a solvent vapor into the liquid phase also resulted in crystals of a solvated cerium(III) halide complex.
1. A process for preparing a cerium halide solvate complex, comprising:
forming a paste of a cerium(III) halide compound and a suitable ionic liquid, the cerium halide being selected from the group consisting of cerium(III) fluoride, cerium(III) chloride, cerium(III) bromide, and cerium(III) iodide,
dissolving at least a portion of the paste into a suitable organic solvent to form either a liquid phase or a solid phase and a liquid phase,
separating any remaining solid phase from the liquid phase, and
forming crystals of the cerium(III) halide solvate complex from the liquid phase.
2. The process of claim 1 , wherein the step of forming crystals of the cerium(III) halide complex comprises allowing vapor from a suitable organic liquid to diffuse into the liquid phase.
3. The process of claim 1 , wherein the step of forming crystals of cerium(III) halide complex from the liquid phase comprises cooling the liquid phase in order to induce the growth of crystals from the liquid phase.
4. The process of claim 1 , wherein the organic solvent is selected from an ether, a carboxylic acid, an ester, an aldehyde, a thiol, a mercaptan, a thioether, a thioester, a nitrile, an amine, a phosphine, and combinations thereof.
5. The process of claim 1 , wherein the organic solvent is selected from diethylether, diisopropylether, diphenylether, formic acid, acetic acid, stearic acid, butyl butyrate, benzyl acetate, ethyl formate, benzaldehyde, butyraldehyde, acetaldehyde, 2-methyl-tetrahydrofuran, methanethiol, butanethiol, tert-butyl mercaptan, dimethylsulfide, diethylsulfide, thioanisole, S-methyl thioacetate, S-tertbutyl thioacetate, S-ethyl thiopropionate, tetrahydrothiophene, 2,6-pyridinedicarhothioic acid, acetronitrile, benzonitrile, glutaronitrile, 2-methylpyridine, 3,5-dimethylpyridine, 4-methylpyridine, tert-butylamine, isopropylamine, triethylphosphine, trimethylphosphine, and combinations thereof.
6. The process of claim 1 , wherein the ionic liquid is 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide.
7. A process for preparing cerium(III) halide solvate complexes, comprising:
combining a suitable ionic liquid with a first cerium(III) halide solvate and a suitable coordinating solvent to form a solid phase and a liquid phase,
separating the solid phase from the liquid phase, and
forming crystals of a second cerium(III) halide solvate from the liquid phase.
8. The process of claim 7 , wherein the first cerium(III) halide solvate complex is CeBr 3 (tetrahydrofuran) 4 and the coordinating solvent is a polyether.
9. The process of claim 7 , wherein the ionic liquid is 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide.
10. The process of claim 8 where the polyether is selected from dimethoxyethane, diglyme, and tetraglyme.