Hydrocarbon solvent solutions of complexes of N-butyllithium and ethyllithium
AssigneeLithium Corporation of America
InventorRobert C. Morrison
Life of this patent
Estimating the term…
Loading patent…
AssigneeLithium Corporation of America
InventorRobert C. Morrison
Estimating the term…
Hydrocarbon, especially aliphatic and/or cycloaliphatic hydrocarbon, solvent solutions of complexes of n-butyllithium and ethyllithium, exemplified by (a) equimolar solutions of n-butyllithium and ethyllithium in n-hexane or cyclohexane, (b) 36 molar % n-butyllithium and 64 mole % ethyllithium in n-hexane or cyclohexane, and (c) 25 mole % n-butyllithium and 75 mole % ethyllithium in n-hexane or cyclohexane. The thermal stability of the complexes of n-butyllithium and ethyllithium in the solutions thereof in hydrocarbon solvents has been found to be outstanding. The hydrocarbon solvent solutions of said complexes, especially where said solvents are aliphatic or cycloaliphatic, have marked advantages over conventionally used hydrocarbon solvent solutions of n-butyllithium as catalysts or initiators in polymerization reactions, telomerization reactions, metalation reactions, halogen-metal interchange reactions, and in the preparation of magnesium alkyls and other organometallics.
In a method of preparing liquid hydrocarbon solutions of complexes of n-butyllithium and ethyllithium in which the ratio of the n-butyllithium to the ethyllithium, on a mole basis, is from about 1:9 to about 9:1, the steps which comprise providing a stirred dispersion of finely divided lithium metal containing a small proportion of sodium metal in a liquid with which the lithium metal is essentially unreactive, discontinuing the stirring and allowing the lithium metal to rise to the top of the mixture, separating out the unreactive liquid and replacing it with a liquid hydrocarbon solvent, gradually adding to said lithium metal dispersion, under conditions of vigorous agitation and in an inert gas atmosphere, a relatively homogeneous mixture of (a) n-butyl chloride or bromide and (b) ethyl chloride or ethyl bromide in predetermined relative proportions to provide the aforesaid solutions containing the complexes in their above-stated mole ratios of the n-butyllithium and ethyllithium, and continuing the reaction at a temperature in the approximate range of about 20.degree. to about 35.degree., under conditions of stirring, until said reaction is at least substantially completed, filtering and washing the reaction muds with a liquid hydrocarbon solvent for said complexes to produce a final clear hydrocarbon solution of said complexes.
In a method of preparing liquid hydrocarbon solutions of complexes of n-butyllithium and ethyllithium in which the ratio of the n-butyllithium to the ethyllithium, on a mole basis, is from about 1:9 to about 9:1, the steps which comprise providing a stirred dispersion of finely divided lithium metal containing a small proportion of sodium metal in a liquid hydrocarbon selected from the group of aliphatic and cycloaliphatic hydrocarbons with which the lithium metal is essentially unreactive, gradually adding simultaneously to said lithium metal dispersion, under conditions of vigorous agitation and in an inert gas atmosphere, (a) n-butyl chloride or bromide and (b) ethyl chloride or bromide in a predetermined relative proportions to provide the aforesaid solutions containing the complexes in their above-stated mole ratios of the n-butyllithium and ethyllithium, and continuing the reaction at a temperature in the approximate range of about 20.degree. to about 35.degree., under conditions of stirring, until said reaction is at least substantially completed, and filtering to produce a solution of said complexes in said hydrocarbon solvent.
In a method of preparing liquid aliphatic and/or cycloaliphatic hydrocarbon solutions of complexes of n-butyllithium and ethyllithium in which the ratio of the n-butyllithium to the ethyllithium, on a mole basis, is from about 1:9 to about 9:1, the steps of which comprise providing a stirred dispersion of finely divided lithium metal containing a small proportion of sodium metal in a liquid with which the lithium metal is essentially unreactive, discontinuing the stirring and allowing the lithium metal to rise to the top of the mixture, separating out the unreactive liquid and replacing it with a liquid hydrocarbon solvent, gradually adding to said lithium metal dispersion, under conditions of vigorous agitation and in an inert gas atmosphere, a relatively homogeneous mixture of (a) n-butyl chloride or bromide, and (b) ethyl chloride or bromide in predetermined relative proportions to provide the aforesaid solutions containing the complexes in their above-stated mole ratios of the n-butyllithium and ethyllithium, and continuing the reaction at a temperature in the approximate range of about 20.degree. to about 35.degree., under conditions of stirring, until said reaction is at least substantially completed, filtering and washing the reaction muds with a liquid hydrocarbon solvent for said complexes to produce a final clear hydrocarbon solution of said complexes.
A composition comprising a clear solution in a liquid hydrocarbon solvent of a complex of n-butyllithium and ethyllithium in which the ratio, on a mole basis, of the n-butyllithium to the ethyllithium is in the range of about 1:9 to about 9:1.
Dependencies are inferred from the claim text.