US4424352A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Palladium(II) bis(hexafluoroacetylacetonate) adducts and their preparation
Assignee: 3M Co
•
Filing: 1980-06-13
•
Granted: 1984-01-03
•
Expires: 2000-06-13
Abstract
Abstract Preparation of palladium(II) bis(hexafluoroacetylacetonate) and adducts derived therefrom are disclosed, said adducts having the formula Pd(F.sub.6 ACAC).sub.2 ·L.sub.n wherein L is a Lewis base selected from certain classes, and n is an integer from 1 to 4. These compounds are useful in preparing catalytic and primer surfaces of elemental palladium.
Inventors
- 👤 Allen R. Siedle
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 19:26
CPC Classifications
C; C07; C07F; C07F15/00; C07F15/0006; C07F15/006; C07F15/0066; B; B01; B01J; B01J23/00; B01J23/38; B01J23/40; B01J23/44; C07C; C07C49/00; C07C49/92; C23; C23C; C23C18/00; C23C18/16; C23C18/18; C23C18/1851; C23C18/1872; C23C18/1875; C23C18/1879; C23C18/20; C23C18/28; C23C18/30
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
117 words
Adducts of palladium(II) bis(hexafluoroacetylacetonate) of the formula Pd(F.sub.6 ACAC).sub.2.L.sub.n wherein F 6 ACAC is the hexafluoroacetylacetonate anion, L is a Lewis base and n is an integer 1 to 4, with the provisos that when n is 1, 2, 3 or 4, L is dimethylethylamine, benzylamine, imidazole, pyrazine, pyrazole, triphenylstibine, benzothiazole, or tert-butylisocyanide, when n is 1, 2, or 3, L is ammonia, methylamine, dimethylamine, or pyridine, when n is 1 or 2, L is trimethylamine, triphenylphosphine, triphenylarsine, 1,4-dithiane, alumina, silica, or aluminosilicates, when n is 4, L is benzoselenazole, when n is 2, L is 1,2-bis(diphenylphosphino)ethane, phenothiazine, or phenoselenazine, and when n is 1, L is phenazine, trimethylpyridine, bis(2-diphenylphosphinoethyl)phenylphosphine, phenoxathiin, tetrathianaphthalene, tetrathiatetracene, benzylmethylsulfide, diethylsulfide, or bis(diphenylphosphino)acetylene.
Claim 2
Dependent Claim
117 words
Adducts of palladium(II) bis(hexafluoroacetylacetonate) of the formula Pd(F.sub.6 ACAC).sub.2.L.sub.n wherein F 6 ACAC is the hexafluoroacetylacetonate anion, L is a Lewis base and n is an integer 1 to 4, with the provisos that when n is 1, 2, 3 or 4, L is dimethylethylamine, benzylamine, imidazole, pyrazine, pyrazole, triphenylstibine, benzothiazole, or tert-butylisocyanide, when n is 1, 2, or 3, L is ammonia, methylamine, dimethylamine, or pyridine, when n is 1 or 2, L is trimethylamine, triphenylphosphine, triphenylarsine, 1,4-dithiane, alumina, silica, or aluminosilicates, when n is 4, L is benzoselenazole, when n is 2, L is 1,2-bis(diphenylphosphino)ethane, phenothiazine, or phenoselenazine, and when n is 1, L is phenazine, trimethylpyridine, bis(2-diphenylphosphinoethyl)phenylphosphine, phenoxathiin, tetrathianaphthalene, tetrathiatetracene, benzylmethylsulfide, diethylsulfide, or bis(diphenylphosphino)acetylene.
Claim 3
Dependent Claim
248 words
Compositions of matter which are adducts of palladium(II) bis(hexafluoroacetylacetonate) selected from the class consisting of Pd(F 6 ACAC) 2 . (CH 3 ) 2 NH! 2 Pd(F 6 ACAC) 2 . (CH 3 ) 2 NH! Pd(F 6 ACAC) 2 .(phenazine) Pd(F 6 ACAC) 2 .(phenoxathiin) Pd(F 6 ACAC) 2 . 2,6-(CH 3 ) 2 C 5 H 3 N! Pd(F 6 ACAC) 2 . (C 6 H 5 ) 3 As! 2 Pd(F 6 ACAC) 2 .(phenoselenazine) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 3 Sb! 4 Pd(F 6 ACAC) 2 .(1,4-C 4 H 8 S 2 ) 2 Pd(F 6 ACAC) 2 .(phenothiazine) 2 Pd(F 6 ACAC) 2 .(benzothiazole) 4 Pd(F 6 ACAC) 2 . (C 2 H 5 ) 2 S! Pd(F 6 ACAC) 2 . (C 6 H 5 CH 2 )(CH 3 )S! Pd(F 6 ACAC) 2 .(alumina) Pd(F 6 ACAC) 2 .(alumina) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 2 PC 2 P(C 6 H 5 ) 2 ! Pd(F 6 ACAC) 2 .(tert-C 4 H 9 NC) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 2 PC 2 H 4 ! 2 PC 6 H 5 Pd(F 6 ACAC) 2 . (CH 3 ) 3 N! 2 Pd(F 6 ACAC) 2 .(1,2- (C 6 H 5 ) 2 P! 2 C 2 H 4 ) 2 Pd(F 6 ACAC) 2 . 2,4,6-(CH 3 ) 3 C 5 H 2 N!.
Claim 4
Dependent Claim
248 words
Compositions of matter which are adducts of palladium(II) bis(hexafluoroacetylacetonate) selected from the class consisting of Pd(F 6 ACAC) 2 . (CH 3 ) 2 NH! 2 Pd(F 6 ACAC) 2 . (CH 3 ) 2 NH! Pd(F 6 ACAC) 2 .(phenazine) Pd(F 6 ACAC) 2 .(phenoxathiin) Pd(F 6 ACAC) 2 . 2,6-(CH 3 ) 2 C 5 H 3 N! Pd(F 6 ACAC) 2 . (C 6 H 5 ) 3 As! 2 Pd(F 6 ACAC) 2 .(phenoselenazine) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 3 Sb! 4 Pd(F 6 ACAC) 2 .(1,4-C 4 H 8 S 2 ) 2 Pd(F 6 ACAC) 2 .(phenothiazine) 2 Pd(F 6 ACAC) 2 .(benzothiazole) 4 Pd(F 6 ACAC) 2 . (C 2 H 5 ) 2 S! Pd(F 6 ACAC) 2 . (C 6 H 5 CH 2 )(CH 3 )S! Pd(F 6 ACAC) 2 .(alumina) Pd(F 6 ACAC) 2 .(alumina) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 2 PC 2 P(C 6 H 5 ) 2 ! Pd(F 6 ACAC) 2 .(tert-C 4 H 9 NC) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 2 PC 2 H 4 ! 2 PC 6 H 5 Pd(F 6 ACAC) 2 . (CH 3 ) 3 N! 2 Pd(F 6 ACAC) 2 .(1,2- (C 6 H 5 ) 2 P! 2 C 2 H 4 ) 2 Pd(F 6 ACAC) 2 . 2,4,6-(CH 3 ) 3 C 5 H 2 N!.
Claim 5
Independent Claim
186 words
A method for preparing adducts of palladium (II) bis(hexafluoroacetylacetonate) of the formula Pd(F.sub.6 ACAC).sub.2.L.sub.n wherein F 6 ACAC is the hexafluoroacetylacetonate anion, L is a Lewis base and n is an integer 1 to 4, with the provisos that when n is 1, 2, 3 or 4, L is dimethylethylamine, benzylamine, imidazole, pyrazine, pyrazole, triphenylstibine, benzothiazole, or tert-butylisocyanide, when n is 1, 2, or 3, L is ammonia, methylamine, dimethylamine, or pyridine, when n is 1 or 2, L is trimethylamine, triphenylphosphine, triphenylarsine, 1,4-dithiane, alumina, silica, or aluminosilicates, when n is 4, L is benzoselenazole, when n is 2, L is 1,2-bis(diphenylphosphino)ethane, phenothiazine, or phenoselenazine, and when n is 1, L is phenazine, trimethylpyridine, bis(2-diphenylphosphinoethyl)phenylphosphine, phenoxathiin, tetrathianaphthalene, tetrathiatetracene, benzylmethylsulfide, diethylsulfide, or bis(diphenylphosphino)acetylene, which method comprises the steps of: (a) reacting the following in a mole ratio appropriate to obtain the desired stoichiometry wherein n has a predetermined value (1) Pd(F 6 ACAC) 2 , (2) a Lewis base as defined above, and (3) optionally, a solvent chosen such that (1) and (2) are soluble therein; and (b) recovering the resulting palladium(II) bis(hexafluoroacetylacetonate) adduct as a solid.
Claim 6
Independent Claim
186 words
A method for preparing adducts of palladium (II) bis(hexafluoroacetylacetonate) of the formula Pd(F.sub.6 ACAC).sub.2.L.sub.n wherein F 6 ACAC is the hexafluoroacetylacetonate anion, L is a Lewis base and n is an integer 1 to 4, with the provisos that when n is 1, 2, 3 or 4, L is dimethylethylamine, benzylamine, imidazole, pyrazine, pyrazole, triphenylstibine, benzothiazole, or tert-butylisocyanide, when n is 1, 2, or 3, L is ammonia, methylamine, dimethylamine, or pyridine, when n is 1 or 2, L is trimethylamine, triphenylphosphine, triphenylarsine, 1,4-dithiane, alumina, silica, or aluminosilicates, when n is 4, L is benzoselenazole, when n is 2, L is 1,2-bis(diphenylphosphino)ethane, phenothiazine, or phenoselenazine, and when n is 1, L is phenazine, trimethylpyridine, bis(2-diphenylphosphinoethyl)phenylphosphine, phenoxathiin, tetrathianaphthalene, tetrathiatetracene, benzylmethylsulfide, diethylsulfide, or bis(diphenylphosphino)acetylene, which method comprises the steps of: (a) reacting the following in a mole ratio appropriate to obtain the desired stoichiometry wherein n has a predetermined value (1) Pd(F 6 ACAC) 2 , (2) a Lewis base as defined above, and (3) optionally, a solvent chosen such that (1) and (2) are soluble therein; and (b) recovering the resulting palladium(II) bis(hexafluoroacetylacetonate) adduct as a solid.
Claim 7
Dependent Claim
251 words
The method according to claim 3 wherein the adducts of palladium(II) bis(hexafluoroacetylacetonate) are selected from the class consisting of Pd(F 6 ACAC) 2 . (CH 3 ) 2 NH! 2 Pd(F 6 ACAC) 2 . (CH 3 ) 2 NH! Pd(F 6 ACAC) 2 .(phenazine) Pd(F 6 ACAC) 2 .(phenoxathiin) Pd(F 6 ACAC) 2 .!2,6-(CH 3 ) 2 C 5 H 3 N! Pd(F 6 ACAC) 2 . (C 6 H 5 ) 3 As)! 2 Pd(F 6 ACAC) 2 .(phenoselenazine) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 3 Sb! 4 Pd(F 6 ACAC) 2 .(1,4-C 4 H 8 S 2 ) 2 Pd(F 6 ACAC) 2 .(phenothiazine) 2 Pd(F 6 ACAC) 2 .(benzothiazole) 4 Pd(F 6 ACAC) 2 . (C 2 H 5 ) 2 S! Pd(F 6 ACAC) 2 . (C 6 H 5 CH 2 )(CH 3 )S! Pd(F 6 ACAC) 2 .(alumina) Pd(F 6 ACAC 2 .(alumina) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 2 PC 2 P(C 6 H 5 ) 2 ! Pd(F 6 ACAC) 2 .(tert-C 4 H 9 NC) 2 Pd(F 6 ACAC) 2 . (C 6 H 5 ) 2 PC 2 H 4 ! 2 PC 6 H 5 Pd(F 6 ACAC) 2 . (CH 3 ) 3 N! 2 Pd(F 6 ACAC) 2 .(1,2- (C 6 H 5 ) 2 P! 2 C 2 H 4 ) 2 Pd(F 6 ACAC) 2 . 2,4,6-(CH 3 ) 3 C 5 H 2 N!.
Claim 8
Dependent Claim
26 words
The method according to claim 3 wherein the solvent is selected from the class consisting of benzene, pentane, hexane, toluene, xylene, dichloromethane, chloroform, methanol, and ethanol.
Claim 9
Dependent Claim
11 words
Adducts according to claim 1 wherein n is equal to 2.
Claim 10
Dependent Claim
11 words
Adducts according to claim 1 wherein n is equal to 3.
Claim 11
Dependent Claim
11 words
Adducts according to claim 1 wherein n is equal to 4.
Claim 12
Dependent Claim
12 words
The method according to claim 3 wherein n is equal to 2.
Claim 13
Dependent Claim
12 words
The method according to claim 3 wherein n is equal to 3.
Claim 14
Dependent Claim
12 words
The method according to claim 3 wherein n is equal to 4.
References Cited (Backward Citations)
US3876675A
Cited
US3770785A
Cited
US3883570A
Cited
US3787462A
Cited
US3946057A
Cited
US3960909A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1987-01-02 | 1987-07-04 | 1988-01-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-01-02 | 1991-07-04 | 1992-01-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-01-02 | 1995-07-04 | 1996-01-03 | $7700.00 | Window Closed / Lapsed |