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US4731203A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for using finely divided highly reactive magnesium

Assignee: Studiengesellschaft Kohle gGmbH
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Filing: 1986-08-12
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Granted: 1988-03-15
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Expires: 2006-08-12
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Abstract

Abstract The present invention relates to a process for preparing a finely divided, highly reactive magnesium from magnesium hydride, magnesium anthracene and/or its derivatives or magnesium butadiene and/or its alkyl or phenyl derivatives, which process is characterized in that the respective magnesium-containing compound is thermally decomposed at a pressure from 10 -6 to 1 bar, the decomposition being carried out in the presence of a co-reactant of a consecutive reaction, or such co-reactant being added only after completion of the precipitation of the magnesium, or in the absence of such co-reactant, the magnesium obtained by said decomposition being isolated as a powder, and to the use of the finely divided, highly reactive magnesium for inserting magnesium into poorly reactive C--X bonds, wherein X denotes heteroatoms such as halogen, oxygen, sulfur, nitrogen, phosphorus, and the resulting organomagnesium compound may be used in a consecutive reaction according to a per se known method, and for the reversible preparation of active magnesium hydride by reaction with molecular hydrogen at a pressure of from 1 to 2 bar and at a temperature of from 150° C. to 250° C.

Inventors

  • 👤 Borislav Bogdanovic

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 02:12
CPC Classifications
B; B82; B82Y; B82Y30/00; B22; B22F; B22F9/00; B22F9/02; B22F9/023; B22F9/16; B22F9/30; C; C01; C01B; C01B6/00; C01B6/04; C07; C07F; C07F3/00; C07F3/02; C22; C22B; C22B26/00; C22B26/20; C22B26/22

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 268 words
In the formation of a compound including a --C--Mg--X moiety wherein X denotes a heteroatom selected from the group consisting of halogen, oxygen, sulfur, nitrogen, phosphorus, by reacting magnesium with a compound containing a poorly reacting --C--X moiety, the improvement which comprises using magnesium produced by thermally decomposing a magnesium-containing compound selected from the group consisting of (i) a magnesium anthracene and/or its derivatives prepared from magnesium and anthracene and/or its alkyl or phenyl derivatives, (ii) a magnesium butadiene and/or its alkyl or phenyl derivatives prepared from magnesium and a conjugated diene having the general formula R 1 --CH═CR 2 --CH═CH--R 3 , wherein R 1 , R 2 and R 3 are the same or different and represent H, a linear or branched alkyl group having from 1 to 6 carbon atoms or a phenyl residue, and (iii) a magnesium hydride-prepared from magnesium and hydrogen either in the presence of homogenous catalysts comprising a halide of a metal of the Subgroups IV to VII of the Periodic System and an organomagnesium compound or a magnesium hydride and in the presence of a polycyclic aromatic or a tertiary amine, after hydrogenating magnesium with magnesium anthracene or magnesium diene, said thermal decomposition taking place at a pressure from 10 -6 to 1 bar and in the absence or presence of an organic aprotic solvent, either the decomposition being carried out in the presence of a co-reactant being added only after completion of the precipitation of the highly reactive magnesium, or in the absence of such co-reactant, the magnesium obtained by said decomposition being isolated as a highly reactive powder.
Claim 2
Dependent Claim 268 words
In the formation of a compound including a --C--Mg--X moiety wherein X denotes a heteroatom selected from the group consisting of halogen, oxygen, sulfur, nitrogen, phosphorus, by reacting magnesium with a compound containing a poorly reacting --C--X moiety, the improvement which comprises using magnesium produced by thermally decomposing a magnesium-containing compound selected from the group consisting of (i) a magnesium anthracene and/or its derivatives prepared from magnesium and anthracene and/or its alkyl or phenyl derivatives, (ii) a magnesium butadiene and/or its alkyl or phenyl derivatives prepared from magnesium and a conjugated diene having the general formula R 1 --CH═CR 2 --CH═CH--R 3 , wherein R 1 , R 2 and R 3 are the same or different and represent H, a linear or branched alkyl group having from 1 to 6 carbon atoms or a phenyl residue, and (iii) a magnesium hydride-prepared from magnesium and hydrogen either in the presence of homogenous catalysts comprising a halide of a metal of the Subgroups IV to VII of the Periodic System and an organomagnesium compound or a magnesium hydride and in the presence of a polycyclic aromatic or a tertiary amine, after hydrogenating magnesium with magnesium anthracene or magnesium diene, said thermal decomposition taking place at a pressure from 10 -6 to 1 bar and in the absence or presence of an organic aprotic solvent, either the decomposition being carried out in the presence of a co-reactant being added only after completion of the precipitation of the highly reactive magnesium, or in the absence of such co-reactant, the magnesium obtained by said decomposition being isolated as a highly reactive powder.
Claim 3
Dependent Claim 40 words
The process according to claim 1, wherein the decomposition of magnesium hydride is carried out in the absence of a solvent under a pressure of from 0.2 to 10 mbar at a temperature of from 250° C. to 300° C.
Claim 4
Dependent Claim 50 words
The process according to claim 1, wherein the decomposition of adducts of magnesium to conjugated dienes of the general formula R 1 --CH═CR 2 --CH═CH--R 3 is carried out in diethylether or dibutylether under a pressure of 1 bar and at a temperature of from -100° C. to +±150° C.
Claim 5
Dependent Claim 51 words
The process according to claim 1, wherein the decomposition of magnesium anthracene 3 THF or an alkyl or phenyl derivative thereof is carried out in the abesence of a solvent under a pressure of from 10 -6 to 10 3 bar at a temperature of from +70° C. to +170° C.
Claim 6
Dependent Claim 54 words
The process according to claim 1, wherein the decomposition of magnesium anthracene 3 THF or an alkyl or phenyl derivative thereof is carried out in an aliphatic, cycloaliphatic or aromatic hydrocarbon or in an open-chain aliphatic ether under a pressure of 1 bar and at a temperature of from -100° C. to +100° C.
Claim 7
Dependent Claim 19 words
The process according to claim 1, wherein said ether is selected from the group consisting of diethylether and dibutylether.
Claim 8
Dependent Claim 29 words
The process according to claim 1, wherein ethyl bromide, 1,2-dichloroethane, 1,2-dibromoethane and magnesium halides are used as promoters or catalysts, respectively, for the decomposition of said thermolabile magnesium compounds.
Claim 9
Dependent Claim 37 words
The process according to claim 1, wherein the decomposition of magnesium hydride is carried out in the absence of a solvent under a pressure of 1 bar at a temperature of from 250° C. to 350° C.
Claim 10
Dependent Claim 73 words
The process according to claim 1, wherein the decomposition of adducts of magnesium to conjugated dienes of the general formula R 1 --CH═CR 2 --CH═CH--R 3 , wherein R 1 , R 2 and R 3 are as defined above, is carried out in an aliphatic, cycloaliphatic or aromatic hydrocarbon or in an open-chain aliphatic ether under a pressure of 1 bar and at a temperature of from -100° C. to +150° C.

References Cited (Backward Citations)

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1991-03-15 1991-09-14 1992-03-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1995-03-15 1995-09-14 1996-03-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1999-03-15 1999-09-14 2000-03-15 $7700.00 Window Closed / Lapsed

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