Systems and methods for preparation of highly reactive alkali metal dendrites for the synthesis of organolithium reagents

Patent metadata

Field	Value
Publication number	US-2024025925-A1
Application number	US-202318224207-A
Country	US
Kind code	A1
Filing date	Jul 20, 2023
Priority date	Jul 20, 2022
Publication date	Jan 25, 2024
Grant date	—

Abstract

Systems and methods for formation of highly reactive alkali dendrites are provided. For example, in some embodiments alkali metals are dissolved in ammonia to form metal electrides after which the ammonia is removed via vacuum to reveal highly activated metal surfaces in the form of crystalline alkali dendrites. The alkali dendrites can mimic powders but have the advantage of being freshly prepared from inexpensive and readily available metal sources. These uniquely activated metals exhibit enhanced reactivity comparatively to similar off the shelf sources of the corresponding metals. For example, the dendrites can have about 100 times greater surface area than conventional metal sources and/or be about 19 times more reactive than powders that serve as the industry standard for the preparation of organometallic compounds. After surface activation, these metals can be used to prepare various organometallic reagents.

First claim

What is claimed is:

1 . A method of forming an alkali dendrite, comprising:
combining an alkali metal with a solvent to form an alloy; and removing the solvent from the alloy to form a alkali dendrite.

2 . The method of claim 1 , wherein combining the alkali metal with the solvent comprises dissolving the alkali metal in the solvent.

3 . The method of claim 1 , wherein the alkali is lithium.

4 . The method of claim 3 , wherein the lithium is a lithium rod. The method of claim 1 , wherein the alkali is one or more of sodium or potassium.

6 . The method of claim 1 , wherein the solvent comprises liquid ammonia.

7 . The method of claim 1 , wherein the solvent comprises one or more of Hexmethylphosphoramide (HMPA) and different degrees of amines.

8 . The method of claim 1 , further comprising keeping a temperature of the alloy substantially constant during the combining step.

9 . The method of claim 8 , further comprising stirring the alloy to evaporate an amount of the solvent from the alloy. The method of claim 9 , wherein an amount of the solvent removed from the alloy can be in approximately a range of about 99% to about 100% with respect to a total amount of the solvent in the alloy.

11 . The method of claim 1 , wherein the solvent is removed by using a vacuum.

12 . The method of claim 1 , wherein a surface area of the alkali dendrite is about 100 times greater than a surface area of a conventional alkali powder.

13 . The method of claim 1 , wherein a surface area of the alkali dendrite is about 2,950 times greater than a surface area of the alkali metal.

14 . The method of claim 1 , wherein a bulk morphology of the alkali dendrite is agglomerated in a dendritic form. The method of claim 1 , wherein a reactivity of the alkali dendrite is about 19 times greater than a reactivity of a conventional alkali powder.

16 . The method of claim 1 , wherein a reactivity of the alkali dendrite is about 199 times greater than a reactivity of the alkali metal.

17 . The method of claim 1 , further comprising reacting the alkali dendrite with an organic halide to form an organometallic reagent.

18 . The method of claim 17 , further comprising synthetically transforming the organometallic reagent by alkylation to generate a yield of about 90% or more

19 . An organo-alkali metal reagent synthesized using the alkali dendrite of claim 1 . A synthetically transformed compound formed from the organometallic reagent of claim 17 .

Assignees

• Texas A & M Univ Sys

Inventors

• Thomas Andy A
• Crockett Michael P
• Aguirre Lupita S
• Jimenez Leonel B
• Hsu Han-Hsiang

Classifications

• C07F1/02 Primary

  Lithium compounds · CPC title

• C07C29/70

  by converting hydroxy groups to O-metal groups {(C07C29/09 takes precedence)} · CPC title

• C07F5/027

  Organoboranes and organoborohydrides · CPC title

• C07C1/328

  the hetero-atom being an alkali metal atom · CPC title

• C07C45/44

  by reduction and hydrolysis of nitriles · CPC title