Preparation of copper(I) chloride
Preparation of copper(I) chloride by reducing copper chloride with hypophosphorous acid
Copper(I) chloride can be conveniently prepared by heating a mixture 40 g of copper sulfate and 20 g sodium hypophosphite in about 500 ml of water to which 30 ml of concentrated hydrochloric acid is added. The copper(I) chloride is deposited and can be purified in the ordinary way.
Preparation of copper(I) chloride by treating copper(II) chloride with metallic copper
42 g of copper(II) chloride are dissolved in 100 ml of hot water containing 32 g metallic copper (granulated or turnings). 200 ml of hydrochloric acid (d=1.175g/ml) is added and the reaction mixture is boiled gently under reflux until the solution becomes colorless. During an experiment additionally a small amount of concentrated hydrochloric acid is added to ensure that solution becomes colorless. This operation lasts one to two hours and when is complete the colorless solution is decanted from the metallic copper into a cylinder filled with cold distilled water. The dilution with water decomposes H3CuCl4 complex and cheesy precipitated copper(I) chloride is allowed to settle, decanted immediately, quickly filtered, washed with alcohol, ether, and dried in a vacuum desiccator. Copper(I) chloride forms heavy white masses, insoluble in water, and oxidizes easily in the air yielding green oxidized product.
Laboratory manual of inorganic preparations, by H. T. Vulte, 73-74, 1895
Preparation of the copper(I) chloride solution for the Sandmeyer reaction
In a 2-liter round-bottomed flask, 125 grams of copper sulfate crystals pentahydrate are dissolved in 400 ml of water by vigorous boiling. In the hot solution 35 grams of sodium chloride are added, which may cause a precipitate of basic copper chloride. A solution of sodium sulfite is prepared from 27 grams of sodium bisulfite, 18 grams of sodium hydroxide and 200 ml of water and this obtained solution is added not too rapidly, to the hot solution containing copper sulfate. When the solution has become decolorized, or nearly so, the content is cooled to room temperature, the colorless cuprous chloride is allowed to settle and decanted the supernatant liquid. The obtained precipitates are washed once by decantation and then dissolved in 175 ml of crude concentrated hydrochloric acid. The flask is stoppered until the solution is to be used.
“Organic Syntheses,” Coll. Vol. I, 163, 1932
Alternatively copper(I) chloride could be prepared from copper(II) chloride – In a 2-liter round-bottomed flask 65 grams of copper(II) chloride (CuCl2 · 2H2O) in 120 ml of crude concentrated hydrochloric acid and to the green solution 25 ml of water and 25 grams of granular (or mossy) zinc are added. The solution is heated at the point of very gentle boiling for one-half hour. The flask is stoppered loosely and set it aside. Just before use the solution is to be cooled in an ice bath.
Travaux Pratiques de Chimie Organique, 189 (1922)
Experiments in Organic Chemistry, L. F. Fieser, 215, 1941
By another method 250 g copper(II) sulfate sodium chloride (120 g), water (500 ml), concentrated hydrochloric acid (1000 g), and copper (130 g) are heated until decolorized. The solution is made up to 2036 g with concentrated hydrochloric acid, then containing about 10% of copper(I) chloride, and after decantation from solid material can be stored if protected from the air. If crystalline copper(I) chloride is wanted, the solution is filtered or decanted, treated with water, and left to cool. Samples that have become partially oxidized during storage can be dissolved in warm hydrochloric acid containing ammonium chloride and heated with copper or sodium sulfite until decolorized.
Ber. Deut. Chem. Ges., 23, 1218 (1890);
Ber. Deut. Chem. Ges. 25, 1086 (1892)
copper (+1) chloride, copper(I) chloride, cuprous chloride, cuprous chloride, 63Cu,1-(37)Cl-labeled, cuprous chloride, 65Cu,1-(35)Cl-labeled, cuprous chloride, 65Cu,1-(37)Cl-labeled
Cuprous chloride, COPPER(I) CHLORIDE, Copper chloride (CuCl), Copper monochloride, Dicopper dichloride, Copper(1+) chloride, 7758-89-6, CuCl, Chlorid medny [Czech], EINECS 231-842-9, Cuprouschloride, Kirticopper, Cuproid, Chlorid medny, Cu-lyt, copper(I)chloride, Copperchloride, copper (I)chloride, copper(I)-chloride, copper (1)chloride, copper(1) chloride, copper-(I) chloride, copper-(I)-chloride, copper (1) chloride, AC1L1XIH, Copper chloride (solution), AC1Q3FL6, Copper(I) chloride solution, CUPROUS CHLORIDE, ACS, KSC492Q9H, 229628_ALDRICH, 651745_ALDRICH, 00664_FLUKA, 08253_FLUKA, 61168_FLUKA, CHEBI:53472, CTK3J2893, MolPort-001-783-708, OXBLHERUFWYNTN-UHFFFAOYSA-M, 61168_SIAL, 212946_SIAL, 224332_SIAL, 256528_SIAL, EINECS 215-704-5, UN2802, RTR-024788, BP-11474, Copper chloride [UN2802] [Corrosive], LS-54862, TR-024788, 12258-96-7, 12622-24-1, 53906-70-0, 53906-71-1, 53906-72-2, 53906-73-3
Copper chloride, Chlorocopper, Copper (I) chloride, copper (+1) chloride, CID62652, cuprous chloride, 63Cu,1-(37)Cl-labeled, cuprous chloride, 65Cu,1-(35)Cl-labeled, cuprous chloride, 65Cu,1-(37)Cl-labeled, C028419, 11093-68-8, 1344-67-8