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inquirychlorocycloocta-1,5-diene(diphenyl-2-pyridylphosphine)rhodium(I)
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
B
{Pd(η3-methylallyl)(2-(diphenylphosphino)pyridine)Cl}
Conditions | Yield |
---|---|
In dichloromethane (N2), after addn. stirred for 2 h, reduced volume, added petroleum ether-diethyl ether (1:1); filtered, washed with diethyl ether, dried in vac., ((C8H12)RhCl)2 recovered from mother liquor; elem. anal.; | A n/a B 95% |
1,5-dicyclooctadiene
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
Conditions | Yield |
---|---|
In ethanol; water react. in ethanol/water in a sealed Teflon container (microwave oven, 2450 MHz, 500 W, 50 sec); | 91% |
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
Conditions | Yield |
---|---|
With cyclooctadiene In ethanol; water in a modified reflux microwave apparatus RhCl3 reacts with cyclooctadiene in EtOH-H2O (5:1) (react. time: 25 min); | 87% |
1,5-dicyclooctadiene
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
Conditions | Yield |
---|---|
In ethanol; water in a microwave oven (Fischer-Porter reaction vessel) at 140°C for 0.5 min; elem. anal.; | 84% |
In ethanol; water under N2 or Ar, reflux of soln. overnight; soln. is cooled, recrystn. from CH2Cl2/hexane; | 82% |
In ethanol A soln. of RhCl*3H2O and COD is refluxed for 45 min until a ppt. sepd. out.; Ppt. is washed with CH3OH, dried at 80°C for 30 min, recrystd. from petroleum ether (60-80°C).; |
dichloro(cycloocta-1,5-diene)palladium (II)
Rh(C8H12)(C5H3N(P(C6H5)2)(OCH3))Cl
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
{Pd(C5H3N(P(C6H5)2)(OCH3))Cl2}2
Conditions | Yield |
---|---|
In dichloromethane (N2); dropwise addn. of the Pd-complex to the Rh-complex in CH2Cl2, stirring for 1 h; the volume of the soln. is reduced, addn. of diethyl ether, filtration, washing (diethyl ether), drying in vac., elem. anal.; | A 71% B 78% |
1,5-dicyclooctadiene
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
Conditions | Yield |
---|---|
In ethanol; water N2-atmosphere; addn. of RhCl3 to soln. of COD, refluxing (5 h), coolingto room temp. (pptn.); collecting, washing (cold H2O and EtOH), drying (1 h in air, then room temp., vac., overnight); | 77% |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
B
RhCl2{C6H3(CH2NMe2)2-o,o'}
Conditions | Yield |
---|---|
In dichloromethane reflux; | A 0% B 0% |
In benzene reflux; | A 0% B 0% |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
zirconium(IV) chloride
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
B
ZrCl3{C6H3(CH2NMe2)2-o,o'}
Conditions | Yield |
---|---|
In dichloromethane instant reaction; no sepn. of metal-contg. products (similar soly.); | |
In benzene instant reaction; no sepn. of metal-contg. products (similar soly.); |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
B
HgCl{C6H3(CH2NMe2)2-o,o'}
Conditions | Yield |
---|---|
With HgCl2 In dichloromethane instant reaction; no sepn. of metal-contg. products (similar soly.); | |
With HgCl2 In benzene instant reaction; no sepn. of metal-contg. products (similar soly.); |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
B
{m-(Me2(H)NCH2)2C6H4}Cl2
Conditions | Yield |
---|---|
With HCl In benzene HCl is bubbled for 1 min through a soln. of Rh complex.; addn. of water, sepn. of layers; evapn. of benzene layer yields (RhCl(COD))2, ammonium salt of aryl compound is obtained from water layer.; | A >99 B >99 |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
rhodium(III)chloride
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
B
RhCl2{C6H3(CH2NMe2)2-o,o'}
Conditions | Yield |
---|---|
In dichloromethane reflux; | A 0% B 0% |
In benzene reflux; | A 0% B 0% |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
iridium (III) chloride
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
Conditions | Yield |
---|---|
In dichloromethane reflux; | A 0% B 0% |
In benzene reflux; | A 0% B 0% |
rhodium{C6H3(CH2NMe2)2-o,o'}(1,5-cyclooctadiene)
tantalum pentachloride
A
di-μ-chloro-bis(1,5-cyclooctadiene)dirhodium
Conditions | Yield |
---|---|
In dichloromethane reflux; | A 0% B 0% |
In benzene reflux; | A 0% B 0% |
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