# US 2014/0194626 A1 · Method for producing amido-zinc halide/alkali- metal halide compounds

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- Number: US 2014/0194626 A1
- Document ID: US20140194626A1
- Status: Published application
- Kind: A1
- Application number: 14/241,690
- Filed: 2012-08-30
- Published: 2014-07-10
- Earliest claimed: 2011-09-02
- Assignees: Rockwood Lithium GmbH
- Inventors: Ulrich Wietelmann; Peter Rittmeyer; Uwe Lischka; Alexander Murso; Florian Kiefer
- Web page: https://patentgrep.com/patent/US20140194626A1

## CPC

- C07F 3/06: Zinc compounds
- C07F 1/02: Lithium compounds
- C07F: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM (metal-containing porphyrins C07D487/22)

## Abstract

The invention relates to a method for producing amido-zinc halides as adducts with alkali-metal halides (R1R2N—ZnY*LiY) in aprotic organic solvents, in which a) a primary or secondary amine dissolved in an aprotic organic solvent is provided, b) a lithium base (RxLi) is added in a metered manner, and c) a ZnY2 is subsequently added.

## Claims

### Claim at position 1

-8. (canceled)

### Claim 9

A method for preparing a compound of formula
R1R2N—ZnY*LiY (I)
comprising the steps of
a) dissolving a primary or secondary amine in an aprotic organic solvent,
b) metering a lithium base (RxLi) into the solvent containing the primary or the secondary amine to form a lithium-containing mixture, and
c) adding ZnY2 to the lithium-containing mixture;
wherein R1 and R2 are independently selected from H, substituted or unsubstituted aryl or heteroaryl containing one or more heteroatoms, a linear, branched, or cyclic substituted or unsubstituted alkyl, alkenyl, alkynyl, or the silyl derivatives thereof; wherein R1 and R2 may together form a cyclic or polymeric structure in which at least one of the radicals R1 and R2 is not H;
Y is selected from the group consisting F; Cl; Br; I; CN; SCN; NCO; HalOz, where z is 3 or 4 and Hal is selected from Cl, Br, and I; NO3; BF4; PF6; H; a carboxylate of the general formula RxCO2; an alcoholate of the general formula ORx; a thiolate of the general formula SRx; R13(O)O2; or SCORx; or SCSRx; OmSRx, where m is 2 or 3; or NOR, where n is 2 or 3; and derivatives thereof; where Rx is a substituted or unsubstituted aryl or heteroaryl containing one or more heteroatoms, a linear, branched, or cyclic substituted or unsubstituted alkyl, alkenyl, alkynyl, or the derivatives thereof, or H.

### Claim 10 (depends on 9)

A method according to claim 9, wherein
a) the amine is provided in a concentration range of 10 to 90% by weight; and
b) a ZnY2 solution in an aprotic organic solvent and R″ Li are simultaneously metered in,
wherein the dosing of the RxLi is started first, and only after 5-10 mol-% RxLi is added is the metering of the ZnY2 solution begun, and during the dosing phase, RxLi and the ZnY2 solution are dosed at different locations in the reaction solution.

### Claim 11 (depends on 9)

A method according to claim 9, wherein the reaction of the amine with the lithium base is carried out continuously in a micro- or meso-flow reactor.

### Claim 12 (depends on 9)

A method according to claims 9, wherein the RxLi is used as a concentrate >95% by weight in an aprotic organic solvent.

### Claim 13 (depends on 9)

A method according to claim 9, wherein the ZnY2 is added in solid form.

### Claim 14 (depends on 13)

A method according to claim 13, wherein Y are independent of one another, or both are Cl, Br, or I and preferably Cl.

### Claim 15 (depends on 9)

A method according to claim 9, wherein the lithium base is n-butyl-Li.

### Claim 16 (depends on 9)

A method according to claim 9, wherein the solvent is selected from the group consisting of a cyclic ether, a linear ether, a branched monoether, a branched polyether, a thioether, an amine and a phosphine, or a derivative thereof which contain at least one heteroatom selected from O, N, S, and P.

### Claim 17 (depends on 9)

A method according to claim 9, wherein the solvent comprises a member from the group consisting of tetrahydrofuran, 2-methyltetrahydrofuran, dibutyl ether, diethyl ether, tert-butylmethyl ether, dimethoxyethane, a dioxane triethylamine, ethyldiisopropylamine, dimethyl sulfide, dibutyl sulfide; cyclic amides, preferably N-methyl-2-pyrrolidone, N-ethyl-2-pyrrolidone, N-butyl-2-pyrrolidone; a cyclic alkane, a cyclic alkene, a linear alkane, a linear alkene, a branched alkane, a branched alkene, a urea derivative, an aromatic hydrocarbon, a heteroaromatic hydrocarbon and an aliphatic hydrocarbon.

### Claim 18 (depends on 9)

A method according to claim 9, wherein the solvent comprises a member from the group consisting of 1,4-dioxane, dichloromethane, 1,2-dichloroethane, CCl4; N,N′-dimethylpropylene urea, benzene, toluene, xylene, pyridine, pentane, cyclohexane, hexane, heptane; hexamethylphosphoric triamide and CS2.

### Claim 19 (depends on 10)

A method according to claim 10, wherein the reaction of the amine with the lithium base is carried out continuously in a micro- or meso-flow reactor.

### Claim 20 (depends on 10)

A method according to claims 10, wherein the RxLi is used as a concentrate >95% by weight in an aprotic organic solvent.

### Claim 21 (depends on 19)

A method according to claims 19, wherein the RxLi is used as a concentrate >95% by weight in an aprotic organic solvent.

### Claim 22 (depends on 10)

A method according to claim 10, wherein the ZnY2 is added in solid form.

### Claim 23 (depends on 11)

A method according to claim 11, wherein the ZnY2 is added in solid form.

### Claim 24 (depends on 12)

A method according to claim 12, wherein the ZnY2 is added in solid form.

### Claim 25 (depends on 9)

A method according to claim 9, wherein the ZnY2 is added in solid form.