Rhodium chloride trihydrate

Catalyst A mixture of 5.26 g of rhodium chloride trihydrate, 0.34 g of palladium chloride, 18 g of carbon (Darco G-60), and 200 ml of water is rapidly stirred and heated to 80°. A solution of lithium hydroxide hydrate (2.7 g) in 10 ml of water is added in one portion and the heating discontinued. Stirring is continued overnight, after which the mixture is filtered and washed with 100 ml of 0.5 % aqueous acetic acid. The product is dried in a vacuum oven at 65°. About 20 g of the catalyst is thus obtained. 

Rhodium chloride trihydrate (1 g, 5.2 mmol) and triphenylphosphine (6 g, 23 mmol) are refluxed in 120 ml of ethanol. The solid tris(triphenylphosphine)rhodium chloride is filtered with suction and washed with ethanol and ether. Yield is 3.5 g (73%). 

The catalyst system for the modem methyl acetate carbonylation process involves rhodium chloride trihydrate [13569-65-8]y methyl iodide [74-88-4], chromium metal powder, and an alumina support or a nickel carbonyl complex with triphenylphosphine, methyl iodide, and chromium hexacarbonyl (34). The use of nitrogen-heterocyclic complexes and rhodium chloride is disclosed in one European patent (35). In another, the alumina catalyst support is treated with an organosilicon compound having either a terminal organophosphine or similar ligands and rhodium or a similar noble metal (36). Such a catalyst enabled methyl acetate carbonylation at 200°C under about 20 MPa (2900 psi) carbon monoxide, with a space-time yield of 140 g anhydride per g rhodium per hour. Conversion was 42.8% with 97.5% selectivity. A homogeneous catalyst system for methyl acetate carbonylation has also been disclosed (37). A description of another synthesis is given where anhydride conversion is about 30%, with 95% selectivity. The reaction occurs at 445 K under 11 MPa partial pressure of carbon monoxide (37). A process based on a montmorillonite support with nickel chloride coordinated with imidazole has been developed (38). Other related processes for carbonylation to yield anhydride are also available (39,40). 

A 500-ml rcund-bottom flask is equipped with a reflux condenser, a gas inlet tube, and a gas outlet leading to a bubbler. The flask is charged with a solution of rhodium (III) chloride trihydrate (2 g) in 70 ml of 95 % ethanol. A solution of triphenylphosphine (12 g, freshly recrystallized from ethanol to remove the oxide) in 350 ml of hot ethanol is added to the flask, and the system is flushed with nitrogen. The mixture is refluxed for 2 hours, following which the hot solution is filtered by suction to obtain the product. The crystalline residue is washed with several small portions of anhydrous ether (50 ml total) affording the deep red crystalline product in about 85% yield. 

Rhodium(III) chloride trihydrate (2 g.) is dissolved in 70 ml. of ethanol (95%) in a 500-ml. round-bottomed flask fitted with gas inlet tube, reflux condenser, and gas exit bubbler. A solution of 12 g. of triphenylphosphine (freshly crystallized from ethanol to remove triphenylphosphine oxide) in 350 ml. of hot ethanol is added and the flask purged with nitrogen. The solution is refluxed for about 2 hours, and the crystalline product which forms is collected from the hot solution on a Buchner funnel or sintered-glass filter. The product is washed with small portions of 50 ml. of anhydrous ether yield 6.25 g. (88% based on Rh). This crystalline product is deep red in color. 

To a solution of 2 g. of rhodium(III) chloride trihydrate in 70 ml. of ethanol is added 12 g. of triphenylphosphine in 250 ml. of hot ethanol. After refluxing until the red solution begins to lighten in color (about 5 minutes), 8 g. of lithium bromide dissolved in 50 ml. of hot ethanol is added and the mixture refluxed for an hour. The orange prisms of the complex are collected by filtration, washed with 50 ml. of anhydrous ether, and dried in vacuum yield 5.1 g. (64% based on rhodium). 

A 200-mL, round-bottomed flask, equipped with a magnetic stir bar, is charged with 1.00 g (3.80 mmol) of rhodium(III) chloride trihydrate (Johnson... 

Tris(ethylenediamine)rhodium(III) chloride, first reported by Werner,1 was prepared by the reaction of sodium hexachloro-rhodate(III) dodecahydrate with ethylenediamine monohydrate. The reaction product, however, contained sodium chloride, which could not be removed by recrystallization,1 probably because of the formation of a double salt. J Jaeger2,8 prepared the compound from rhodium (III) chloride trihydrate and 50 % aqueous ethylenediamine. Gillard, Osborn, and Wilkinson4 carried out the reaction of rhodium(III) chloride... 

Rhodium(III) chloride trihydrate (26.3 g., 0.10 mole) is placed in a 100-ml. round-bottomed flask which is then fitted with a condenser.. The flask is immersed in an ice bath, and an ice-cold mixture of 27 ml. (0.33 mole) of ethylenediamine monohydrate and 25 ml. of water is added through the condenser. The mixture should be added very carefully at first, and the whole addition should take at least 5 minutes as the initial reaction is very vigorous. The ice bath is removed (but kept at hand for controlling the reaction, if necessary). The reaction mixture is heated very carefully and finally refluxed until the rhodium chloride is dissolved (10-15 minutes). The solution is cooled for 15 minutes before 25 ml. of ethanol is added through the condenser. The mixture is boiled until the precipitate formed has redissolved, and the yellow solution is then allowed to stand at room temperature for 2 hours. During standing, white, needlelike crystals separate. Finally the mix-... 

Tris(ethylenediamine)rhodium(III) chloride trihydrate (11.10 g., 0.025 mole) and 5.63 g. (0.0375 mole, 50% excess) of (+)-tartaric acid and 3.15 g. (0.075 mole) of LiOH-H20 are placed in a 100-ml. conical flask and dissolved in 25 ml. of boiling water. When a clear solution has formed, the solution is allowed to cool somewhat by standing for 5 minutes. Fifteen milliliters of ethanol is then added, and the solution is allowed to stand for 3 hours at room temperature with occasional shaking. During standing, white crystals of the tartrate double salt separate. The precipitate is filtered, washed with three 10-ml. portions of a 1 1 mixture of ethanol and water, and dried in air. The yield is approximately 8.3 g. 

A 1000-mL two-necked flask equipped with a frit diffuser tube (CO inlet), a two-way stopcock (CO outlet) and a magnetic stirring bar is used as the reactor. Rhodium trichloride trihydrate (2.63 g, 10.0mmol) and potassium chloride (2.24 g, 30.0 mmol) are dissolved in 500 mL of water in the reactor. Copper powder (2g) is added, and the solution is bubbled with CO for 12 h with stirring at room temperature. To the resultant solution is added 2.94 g of trisodium citrate dihydrate, and stirring is continued for an additional 12 h under a CO atmosphere. The precipitate is collected under N2 and extracted with CO saturated hexane five times. Dodecacarbonyltetrarhodium (1.46g, 1.96 mmol) is obtained by evaporation of the hexane on a rotary evaporator (78% yield). IR (in hexane) 2072, 2070, 2043, and 1886cm . ... 

The chloride is obtainable also as a water-sol hydrate with variable amounts of water. Prepn of trihydrate Anderson, Basolo, Inorg. Syn. 7, 214 (1963). Similar to the chlorides of other platinum group metals, rhodium chloride readily forms double salts with alkali chlorides. 

Rhodium (III) chloride trihydrate (2 g) is dissolved in 70 mL of ethanol (95%) in a 500 mL round-bottomed flask fitted with gas inlet tube, reflux condenser, and gas exit bubbler. A solution of 12 g of triphenylphosphine... 

The commercially available rhodium(III) chloride trihydrate (RhCl3-3H20) complex has been found to be the best starting material for the preparation of various Rh compounds. Additionally, this complex can also be prepared using known methods. An alternative starting material is anhydrous rhodium(III) chloride, but it is insoluble in many conventional solvents, which often leads to low yields. 

A hot solution of triphenylphosphine (12 g, 46 mmol) in ethanol (350 mL) was added to a solution of rhodium(III) chloride trihydrate (2.0 g, 7.6 mmol) in 95% ethanol (70 mL) in a 500-mL, round-bottomed flask fitted with nitrogen inlet, reflux condenser, and a gas exit bubbler. After heating the solution at reflux for 2 h, the hot solution was filtered to give the crystalline product, which was washed with anhydrous ether and dried under vacuum to yield RhCl(PPh3)3 (6.25 g, 88% based on Rh) as an orange-red solid. ... 

A gas washing bottle was charged with pulverized rhodium(lll) chloride trihydrate (11.0 g, 0.042 mol).The apparatus was then flushed with CO and lowered into a pre-heated oil bath at 100 °C. 

A 100-mL, two-necked, round-bottomed flask was fitted with a reflux condenser connected to a nitrogen bubbler. The flask was charged with rhodium(III) chloride trihydrate (2.0 g, 7.6 mmol) and sodium carbonate decahydrate (2.2 g, 7.7 mmol) under nitrogen. The degassed ethanol-water (5 1, 3 mL) and 1,5-cyclooctadiene (cod) (3 mL) were added and the mixture was then heated at reflux with stirring for 18 h. The mixture was cooled and immediately filtered and the product was washed with pentane and then with methanol-water (1 5). The product was dried in vacuo to afford [Rh(C8Hi2)Cl]2 (1.67 g, 94%) as a yellow-orange solid. 

Preparative Method rhodium(III) chloride trihydrate (10 g, 0.042 mol) and pentamethylcyclopentadiene (6 g, 0.044 mol) were placed in a 500 mL round-bottomed flask with condenser and dissolved in reagent-grade methanol (300 mL). The solution was heated under reflux under a N2 atmosphere for 48 h. The resulting dark red precipitate was Altered and washed with diethyl ether and dried under reduced pressure. ... 

Formula RhCE MW 209.26 forms a trihydrate RhCl3 3H20 Synonyms rhodium trichloride rhodium(III) chloride... 

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