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. 

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. 

Gold Acid Chloride Trihydrate Potassium Carbonate... 

Iridium phthalocyanine (Pclr) is prepared by the reaction of 2-cyanobenzamide with irid-ium(III) chloride trihydrate at 280°C.284... 

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). 

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%). 

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... 

S-(2,3,4,6-Tetra-0-acetylglucopyranosyl)thiopseudourea hydrobromide Gold acid chloride trihydrate Potassium carbonate... 

A) Triethylphosphine gold chloride A solution of 10.0 g (0.08 mol) of thiodiglycol in 25 ml of ethanol is mixed with a solution of 15.76 g (0.04 mol) of gold acid chloride trihydrate in 75 ml of distilled water. When the bright orange-yellow solution is almost colorless, it is cooled to -5°C and an equally cold solution of 5.0 g (0.0425 mol) of triethylphosphine in 25 ml of ethanol is added dropwise to the stirred solution. After the addition is complete, the cooled mixture is stirred for Vi hour. Solid that separates is removed and the filtrate is concentrated to about 30 ml to yield a second crop. The combined solid is washed with aqueous-ethanol (2 1) and recrystallized from ethanol by adding water to the cloud point. The product is obtained as white needles, MP 85° to 86°C. 

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. 

Tris(ethylenediamine)chromium(III) chloride trihydrate (39.3 g., 0.10 mole) and 22.5 g. (0.15 mole) of (+)-tartaric acid, and a magnetic stirring bar, are placed in a 400-ml. beaker. A 100-ml. volume of water is added, and the mixture is dissolved with stirring. Immediately after the dissolution, 12.6 g. (0.30 mole) of IiOH-H20 is added with continued stirring. The hydroxide dissolves, and shortly after a yellow crystalline precipitate is formed. About 5 minutes after the addition of the hydroxide, 100 ml. of ethanol is added dropwise with continued stirring during a 15-minute period. The precipitate is filtered, and the filtrate is run directly into a mixture of 15 ml. (0.18 mole) of 12 M HC1 and 600 ml. of absolute ethanol. From this system a finely crystalline precipitate of impure (—)D-chloride separates out. The filter flask is replaced, and the crystals are washed with three 50-ml. portions of a 1 1 mixture of ethanol and water and dried in air. (Yield is 27-28 g.) The precipitate of (—)D-chloride from the filtrate is filtered, washed with three 50-ml. portions of ethanol, and dried in air. (Yield is 13-14 g.)... 

Lundgren J-O, Olovsson I (1967) Hydrogen bond studies.XVI. The crystal structure of chloride trihydrate. Acta Crys 23 971-976... 

Struniewicz C, Milet A, Sadlej J, Moszynski R (2002) Theoretical study of the hydrogen chloride trihydrate. Int J Quantum Chem 90 1151-1162... 

Cycloaddition of vinylketenes, produced in situ from the dehydrohalogenation of appropriately substituted unsaturated acid chlorides, with alkenes provides a convenient source of 2-vinyl-cyclobutanones. Oxidation with ruthenium(III) chloride trihydrate gave the corresponding P-oxo acid, which by treatment with oxalyl chloride and diazomethane, successively, led to the desired 2-(2-diazoacetyl)cyclobutanones. These diazo ketones are thermally labile and rearrange upon brief heating in refluxing xylene to give the spiro[cyclopropane-l,5 -furan-2 (5 i/)-ones] 2 (Table 2). ... 

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