Process for the preparation of alkyllithium compounds
View Patent ↗A process for preparing alkyllithium compounds by reacting a sodium-lithium alloy with alkyl halides at temperatures of about 50 to 125° C.
1. A process for producing alkyllithium compounds in high yields of at least about 90% and high purity by reacting under reflux conditions in a liquid hydrocarbon solvent which refluxes at temperatures between about 50° C. and 125° C., such solvent being selected from liquid saturated aliphatic hydrocarbons containing 5 to 12 carbon atoms, saturated liquid cycloaliphatic hydrocarbons containing 5 to 12 carbon atoms and liquid aromatic hydrocarbons containing 6 to 12 carbon atoms and mixtures thereof, an alkyl halide containing 3 to 16 carbon atoms with metal particles of less than about 300 microns in size, and subsequently recovering the alkyllithium compound, in which the improvement consists of conducting the reaction using metal particles of a lithium-sodium alloy which comprises at least about 15 percent by weight of sodium.
2. The process of claim 1 , wherein the lithium-sodium alloy comprises about 34% by weight sodium and about 66% by weight lithium.
3. The process of claim 1 , wherein the alkyl halide is an alkyl chloride containing from about 3 to about 16 carbon atoms.
4. The process of claim 1 , wherein the alkyl halide is butyl chloride.
5. The process of claim 1 , wherein the solvent is hexane and the reaction temperature is between about 68-80° C.
6. The process of claim 1 , wherein the solvent is heptane and the reaction temperature is between about 99-110° C.
7. The process of claim 1 , wherein the solvent is cyclohexane and the reaction temperature is between about 80-90° C.
8. The process of claim 1 , wherein the solvent is toluene and the reaction temperature is between about 110-120° C.
9. The process of claim 1 , wherein the reaction time is about 70 minutes.
10. The process of claim 5 , wherein the alkyl halide is an alkyl chloride containing from 3 to 16 carbon atoms.
11. The process of claim 10 , wherein the alkyl halide is butyl chloride.
12. The process of claim 6 , wherein the alkyl halide is an alkyl chloride containing from 3 to 16 carbon atoms.
13. The process of claim 12 , wherein the alkyl halide is butyl chloride.
14. The process of claim 7 , wherein the alkyl halide is an alkyl chloride containing from 3 to 6 carbon atoms.
15. The process of claim 14 , wherein the alkyl halide is butyl chloride.
16. The process of claim 8 , wherein the alkyl halide is an alkyl chloride containing from 3 to 16 carbon atoms.
17. The process of claim 16 , wherein the alkyl halide is butyl chloride.
18. The process of claim 9 , wherein the alkyl halide is an alkyl chloride containing from 3 to 16 carbon atoms.
19. The process of claim 18 , wherein the alkyl halide is butyl chloride.