US4055582A
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Synthesis of nickel and palladium organophosphorus complexes
Assignee: Phillips Petroleum Co
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Filing: 1976-05-10
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Granted: 1977-10-25
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Expires: 1996-05-10
Abstract
Abstract A process is disclosed comprising reacting at least one compound of the formula RMX(PR 3 ) 2 and at least one compound of the formula APR 2 to produce at least one composition which can be represented by the formula M(PQ 3 ) n , wherein M is palladium or nickel; X is a halogen; A is an alkali metal; each R is individually selected from the group consisting of suitable aliphatic hydrocarbyl radicals, halosubstituted aliphatic hydrocarbyl radicals, aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, halosubstituted aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, hydrocarbyloxy radicals, and halosubstituted hydrocarbyloxy radicals, each Q is individually selected from any R contained in the reactants; each PR 3 may be the same or different; each PQ 3 may be the same or different; the molar ratio of each different PQ 3 to M can be any rational number such that the sum of the molar ratios of the different PQ 3 's equals n; and n equals 3 when M is palladium or 4 when M is nickel.
Inventors
- 👤 Darryl R. Fahey
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 01:38
CPC Classifications
C; C07; C07F; C07F15/00; C07F15/04; C07F15/045; C07F15/0006; C07F15/006; C07F15/0066
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
200 words
A process comprising reacting at least one compound of the formula RMX(PR 3 ) 2 with at least one compound of the formula APR 2 in the presence of a diluent under reaction conditions sufficient to produce at least one composition which can be represented by the formula M(PQ 3 ) n , wherein M is palladium or nickel; X is a halogen; A is an alkali metal; each R is individually selected from the group consisting of suitable aliphatic hydrocarbyl radicals, halosubstituted aliphatic hydrocarbyl radicals, aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, halosubstituted aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, hydrocarbyloxy radicals, and halosubstituted hydrocarbyloxy radicals, each Q is individually selected from any R contained in the reactants; each PR 3 may be the same or different; each PQ 3 may be the same or different; the molar ratio of each different PQ 3 to M can be any rational number such that the sum of the molar ratios of the different PQ 3 's equals n; and n equals 3 when M is palladium or 4 when M is nickel.
Claim 2
Dependent Claim
200 words
A process comprising reacting at least one compound of the formula RMX(PR 3 ) 2 with at least one compound of the formula APR 2 in the presence of a diluent under reaction conditions sufficient to produce at least one composition which can be represented by the formula M(PQ 3 ) n , wherein M is palladium or nickel; X is a halogen; A is an alkali metal; each R is individually selected from the group consisting of suitable aliphatic hydrocarbyl radicals, halosubstituted aliphatic hydrocarbyl radicals, aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, halosubstituted aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, hydrocarbyloxy radicals, and halosubstituted hydrocarbyloxy radicals, each Q is individually selected from any R contained in the reactants; each PR 3 may be the same or different; each PQ 3 may be the same or different; the molar ratio of each different PQ 3 to M can be any rational number such that the sum of the molar ratios of the different PQ 3 's equals n; and n equals 3 when M is palladium or 4 when M is nickel.
Claim 3
Dependent Claim
15 words
A process according to claim 1 wherein each R contains 1 to 12 carbon atoms.
Claim 4
Dependent Claim
56 words
A process according to claim 2 wherein each R is individually selected from the group consisting of alkyl, aryl wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, alkoxy, aryloxy, alkaryl, alkynyl, haloalkyl, haloaryl wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, alkaryl, aralkyl, and alkadienyl radicals.
Claim 5
Dependent Claim
56 words
A process according to claim 2 wherein the molar ratio of APR 2 to RMX(PR 3 ) 2 is in the range of about 0.5:1 to about 1.5:1, the temperature is in the range of about -50° to about 200° C an the pressure is such that the diluent is essentially maintained in the liquid phase.
Claim 6
Dependent Claim
23 words
A method according to claim 4 wherein M is nickel and each said APR 2 is employed in the form of an etherate.
Claim 7
Dependent Claim
22 words
A method according to claim 5 wherein at least one transhalo(phenyl)bis(triethylphosphine)nickel(II) is reacted with at least one alkali metal diphenylphosphide diethyl etherate.
Claim 8
Dependent Claim
17 words
A method according to claim 6 wherein trans-bromo(phenyl)bis(triethylphosphine)nickel(II) is reacted with an alkali metal diphenylphosphide diethyl etherate.
Claim 9
Dependent Claim
19 words
A method according to claim 7 wherein the alkali metal of the alkali metal diphenylphosphide diethyl etherate is lithium.
Claim 10
Dependent Claim
37 words
A method according to claim 8 wherein the molar ratio of transbromo(phenyl)bis(triethylphosphine)nickel(II) to lithium diphenylphosphide diethyl etherate is about 1:1, the temperature is about 0° C, and the reaction is conducted under an atmosphere of inert gas.
Claim 11
Dependent Claim
12 words
A method according to claim 9 wherein tris(triethylphosphine)(triphenylphosphine)nickel is produced and recovered.
Claim 12
Dependent Claim
88 words
A method according to claim 5 wherein at least one compound of the formula PR 3 is also included as a reactant, wherein each R is individually selected from the group consisting of suitable aliphatic hydrocarbyl radicals, halosubstituted aliphatic hydrocargyl radicals, aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, halosubstituted aromatic hydrocarbyl radicals wherein at least one carbon adjacent the radical carbon has a hydrogen substituent, hydrocarbyloxy radicals, and halosubstituted hydrocarbyloxy radicals, said radicals having 1 to 12 carbon atoms.
Claim 13
Dependent Claim
21 words
A method according to claim 11 wherein each R is individually selected from the group consisting of alkyl or aryl radicals.
Claim 14
Dependent Claim
29 words
A method according to claim 12 wherein the molar ratio of PR 3 to said RMX(PR 3 ) 2 is in the range of about 0.5:1 to about 1.5:1.
Claim 15
Dependent Claim
26 words
A method according to claim 13 wherein at least one transhalo(phenyl)bis(triethylphosphine)nickel(II) and at least one alkali metal diphenylphosphide etherate are reacted in the presence of triethylphosphine.
Claim 16
Dependent Claim
33 words
A method according to claim 14 wherein trans-bromo(phenyl)bis(triethylphosphine)nickel(II) and lithium diphenylphosphide diethyl etherate are reacted in the presence of triethylphosphine at a temperature of about 0° C under an atmosphere of inert gas.
Claim 17
Dependent Claim
12 words
A method according to claim 15 wherein tris(triethylphosphine)(triphenylphosphine)nickel(0) is produced and recovered.
Claim 18
Dependent Claim
26 words
A method according to claim 13 wherein at least one transhalo(phenyl)bis(triphenylphosphine)nickel(II) and at least one alkali metal diphenylphosphide etherate are reacted in the presence of triphenylphosphine.
Claim 19
Dependent Claim
33 words
A method according to claim 17 wherein trans-bromo(phenyl)bis(triphenylphosphine)nickel(II) and lithium diphenylphosphide diethyl etherate are reacted in the presence of triphenylphosphine at a temperature of about 0° C under an atmosphere of inert gas.
Claim 20
Dependent Claim
12 words
A method according to claim 18 wherein tetrakis(triphenylphosphine)nickel(0) is produced and recovered.
Claim 21
Dependent Claim
21 words
A method according to claim 5 wherein each R is individually selected from the group consisting of alkyl or aryl radicals.
Claim 22
Dependent Claim
23 words
A method according to claim 4 wherein M is palladium and each said APR 2 is employed in the form of an etherate.
Claim 23
Dependent Claim
22 words
A method according to claim 21 wherein at least one transhalo(phenyl)bis(triethylphosphine)palladium(II) is reacted with at least one alkali metal diphenylphosphide diethyl etherate.
Claim 24
Dependent Claim
17 words
A method according to claim 22 wherein trans-bromo(phenyl)bis(triethylphosphine)palladium(II) is reacted with an alkali metal diphenylphosphide diethyl etherate.
Claim 25
Dependent Claim
19 words
A method according to claim 23 wherein the alkali metal of the alkali metal diphenylphosphide diethyl etherate is lithium.
Claim 26
Dependent Claim
53 words
A method according to claim 24 wherein the temperature is about 0° C, the reaction is conducted under an atmosphere of inert gas, and a composition of the formula Pd(PEt 3 ) 1 .9 (PPh 3 ) 1 .1 is produced and recovered wherein PEt 3 is triethylphosphine and PPh 3 is triphenylphosphine.
Claim 27
Dependent Claim
29 words
A composition of matter having the average formula of Pd(PEt 3 ) 1 .9 (PPh 3 ) 1 .1 wherein PEt 3 is triethylphosphine and PPh 3 is triphenylphosphine.
Claim 28
Dependent Claim
29 words
A composition of matter having the average formula of Pd(PEt 3 ) 1 .9 (PPh 3 ) 1 .1 wherein PEt 3 is triethylphosphine and PPh 3 is triphenylphosphine.
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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) | 1980-10-24 | 1981-04-25 | 1981-10-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-10-24 | 1985-04-25 | 1985-10-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-10-24 | 1989-04-25 | 1989-10-25 | $7700.00 | Window Closed / Lapsed |