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inquirydirhodium(II) tetraacetate
Conditions | Yield |
---|---|
In water redn. of Rh2(CH3CO2)4NO3 in aq. and alcoholic solns.; |
Conditions | Yield |
---|---|
In melt Rh complex and pyridine compd. are heated in a N2 atmosphere to 150°C for 72 h, prolonged heating; vac. sublimation at 90°C; elem. anal.; | 90% |
Conditions | Yield |
---|---|
In acetone byproducts: rhodium; mixing finely divided Rh2Ac4 with concd. H2SO4, stirring thoroughly, keeping for 1 h at 140°C, dissolving the sinter in acetone, filtn.,addn. of pyridine; filtn., washing with acetone, ethanol, and ether, elem. anal.; | 60% |
Conditions | Yield |
---|---|
In water treating Rh2Ac4 with H2SO4, heating for 3-4 h to 140°C, dissolving in acetone, filtn., evapn. to dryness, dissolving in water, addn., ofCs2CO3, passing argon through the soln.; evapn., dissolving in water, salting-out with alcohol, filtn., washing with alcohol and ether, elem. anal.; | 50% |
Conditions | Yield |
---|---|
byproducts: rhodium; mixing Rh2Ac4 with H2SO4, keeping for 1 h at 140°C, treating with H2SO4 at 140°C for 10 h, addn. of water, filtn., addn. of Na2CO3 soln., evapn., treating with H2SO4 at 140°C for 10-12 h, dissolving in water, addn. of Na2CO3 soln.; filtn., washing with water, alcohol, and ether, elem. anal.; | 40% |
dirhodium(II) tetraacetate
2,7-di-t-butyl-9,9-dimethyl-4,5-xanthenedicarboxylic acid
C
Rh4(CH3COO)4((COOC6H2C4H9)2OC(CH3)2)2
Conditions | Yield |
---|---|
In further solvent(s) ligand and Rh-complex were stirred in N,N-dimethylaniline at 140°C for 24 h, cooled, diluted in CH2Cl2, MeCN was added under Ar; washed with aq. HCl, water, organic layer was dried, evapd., chromd. acetone-CH2Cl2; elem. anal.; | A 33% B 7% C 40% |
dirhodium(II) tetraacetate
2,7-di-t-butyl-9,9-dimethyl-4,5-xanthenedicarboxylic acid
C
Rh4(CH3COO)4((COOC6H2C4H9)2OC(CH3)2)2
Conditions | Yield |
---|---|
In further solvent(s) ligand and Rh-complex were stirred in N,N-dimethylaniline at 140°C for 24 h, cooled, diluted in CH2Cl2 under Ar; washed with aq. HCl, water, organic layer was dried, evapd., chromd. MeOH-CH2Cl2; elem. anal.; | A 5% B 32% C 24% |
dirhodium(II) tetraacetate
trimethylsilyl bromide
Conditions | Yield |
---|---|
In toluene (Ar); Rh compd. and Me3SiBr in toluene were stirred at ambient temp. for 14 h; formed pptn. was filtered off, filtrate was allowed to evaporate slowly in air, red crystals were obtained after 1 week; | 6% |
dirhodium(II) tetraacetate
Rh2(CH3COO)4(CO)
Conditions | Yield |
---|---|
With carbon monoxide In further solvent(s) reaction at 1 atm CO and 0°C in C2H4Cl2; UV; |
Conditions | Yield |
---|---|
byproducts: rhodium; mixing finely divided Rh2Ac4 with concd. H2SO4, stirring thoroughly, keeping for 1 h at 140°C, finely dividing the resulting sinter, treating with H2SO4 at 140°C for 10 h, dissolving in water, filtn., neutralisation with concd. K2CO3 soln.; filtn., washing with water, alcohol, and ether, elem. anal.; | 20-30 |
Conditions | Yield |
---|---|
In acetone byproducts: rhodium; mixing finely divided Rh2Ac4 with concd. H2SO4, stirring thoroughly, keeping for 1 h at 140°C, dissolving the sinter in acetone, filtn.,addn. of an acetone soln. of thiourea; filtn., washing with acetone and ether, elem. anal.; | 90-95 |
dirhodium(II) tetraacetate
Conditions | Yield |
---|---|
With nitric acid In nitric acid reaction of concd. HNO3 with Rh2(CH3CO2)4; elem. anal.; |
heptafluorobutyric Acid
dirhodium(II) tetraacetate
dirhodium(II) perfluorobutyrate
Conditions | Yield |
---|---|
With perfluorobutiric anhydride refluxed for 15 min, N2 atm.; evapn., cooling at -20°C for 24 h, filtration, washing a residuewith cold pentane, recrystn. (benzene), drying at 100°C in vac. over NaOH for 12 h; elem. anal.; |
Conditions | Yield |
---|---|
In hydrogenchloride under N2; soln. of Mo cluster in toluenesulfonic acid was mixed with soln. of Rh complex in 2 M HCl (prepared with heating); mixt. was heated for 6 h; TsOH was added, chromy.; UV, elem. anal.; |
Conditions | Yield |
---|---|
at 130℃; for 12h; Inert atmosphere; |
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