II Chloride 2-Hydrate

glass tube D, fitted at each end with a ground-glass joint and having sealed at the center a medium-porosity sintered-glass disk E, connects the two flasks. 

Iron (II) chloride 2-hydrate, so prepared, is white with a very pale green tint. The crystal form is monoclinic. The compound is slowly oxidized in air, but its freshly 

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Naphthalenedithiol can be prepared by adding 1,5-naph-thalenedisulfonyl chloride to an ethanol solution of tin (II) chloride 2-hydrate saturated with hydrogen chloride.6 An 80% yield of the crude dithiol melting at 103° was previously reported using zinc dust and sulfuric acid.7... 

Twelve grams of pure tin are dissolved in a mixture of 50g of concentrated hydrochloric acid and 2.5ml of 8M nitric add. Alternatively, 23g of tin (II) chloride 2-hydrate may be used, omitting the nitric add. The solution is diluted to 2 liters with boiling water and hydrogen sulfide passed in under the hood until the light-brown precipitate of stannous sulfide settles well. The solid is suction-filtered, washed with 100ml of hot water followed by 50ml of acetone, and dried at 100°G. 

Five grams of nickel(II) chloride 6-hydrate and 12.1 g. of tris(ethylenediamine)nickel(II) chloride 2-hydrate J are gently refluxed for 5 minutes with a mixture of 47.5 ml. of methanol and 2.5 ml. of water, shaking at first until all the salts are dissolved. A beautiful deep blue solution results. This is filtered by gravity while still warm into a 400-ml. beaker, and the flask and paper are washed once with 5 ml. of hot methanol. Seed crystals are obtained by adding 3 to 4 ml. of acetone slowly to 2 to 3 ml. of the blue solution and scratching or shaking until crystals form the separation of two liquid phases indicates the addition of too much acetone and makes the formation of crystals difficult. 

TRIS (ETHYLENEDIAMINE) NICKEL (II) CHLORIDE 2-HYDRATE TRIS (PROPYLENEDIAMINE) NICKEL (II) CHLORIDE 2-HYDRATE... 

For the preparation of tris(ethylenediamine)nickel(II) chloride 2-hydrate, 28 g. of 70% aqueous ethylenediamine is added to a solution of 23.8 g. (0.1 mol) of NiCl2 6H20 in 100 to 150 ml. of water. The purple solution is filtered to remove the small amount of hydrous iron oxide which precipitates and is then evaporated to a volume of 60 to 70 ml. on a steam bath. Two drops of ethylenediamine are added, and the solution is cooled in an ice bath. The orchid-colored crystals that form are collected by suction, washed twice with 95 % ethanol, and air-dried. The yield is 28.6 g. (80%). Several more grams may be recovered from the mother liquor by adding ethanol and cooling. Anal. Calcd. for [Ni(C2H8N2)3]Cl2-2H20 Ni, 16.97% Cl, 20.50%. Found Ni, 16.87% Cl, 20.48%. 

For the preparation of tris(propylenediamine)nickel(II) chloride 2-hydrate, the above procedure is followed substituting 90% aqueous propylenediamine for the 70% ethyl-... 

Tris (ethylenediamine) cobalt (III) ion, resolution of, through chloride dextro-tartrate, 6 183 synthesis of dextro-, through chloride dextro-tartrate, 6 186 Tris (ethylenediamine) nickel (II) chloride, 2-hydrate, 6 200 Trisilane, octachloro-, 1 44 Trisilicon octachloride, 1 44 Tris(2,4-pentanedionato)aluminum, 2 25... 

A 1.06-g. (0.00622 mole) quantity of copper(II) chloride 2-hydrate is dissolved in 5 ml. of absolute ethanol. This solution is added drop by drop with stirring to an aqueous solution of the ligand, 2.00 g. (0.0124 mole) in 25 ml. of water. As the copper solution is added to the ligand solution, a deep blue color develops. After 3 hours, large crystals form, and after 24 hours, the deep blue crystals are filtered off, using a 30-ml. medium-porosity funnel. The crystals are washed on the crucible with two portions of acetone, two portions of dry ether, and are air-dried. The yield is 1.73 g. [61%, based on the copper(II) chloride]. Anal. Calcd. for Cu(C6H22Nio04)Cl2 Cu, 13.91 C, 21.04 H, 4.85 N, 30.66 Cl, 15.52. Found Cu, 13.75 C, 20.99 H, 4.70 N, 30.90 Cl, 15.79. 

Purification of Europium. An acetate solution obtained from 20 g. of europium(III) oxide (>99% pure) was treated with 260 ml. of 0.3% sodium amalgam, added in three separate equal portions. The resulting amalgam contained all but 0.09 g. of the europium. Treatment of the amalgam with 100 ml. of 10 M hydrochloric acid caused complete precipitation of europium(II) chloride 2-hydrate. Removal of the product followed by washing with ice-cold 10 M hydrochloric acid and ultimate conversion to euro-pium(III) oxide gave a recovery of spectroscopically pure europium in excess of 90%. 

Aquopentammine- and acido-pentamminechromium(III) salts, synthesis 36 Tripotassium enneachloroditung-state(III), synthesis 38 Uranium(IV) chloride, synthesis 39 Uranium(III) chloride, synthesis 40 Uranyl chloride, synthesis 41 Iron(II) chloride 2-hydrate, synthesis 48... 

Tetrahydrofuran is purified by distillation from LiAlH4.21 Anhydrous tin(II) chloride may be obtained by dehydrating tin (II)-chloride 2-hydrate according to a procedure from Organikum, p. 697, (Deutscher Verlag der Wissenschaften, Berlin, 1969). In a 300-ml. beaker, 102 g. of acetic anhydride and 113 g. of tin (II) chloride 2-hydrate are mixed. Dehydration is so exothermic that the anhydride begins to boil. ( Caution. Fume hood.) At the same time, the anhydrous salt precipitates. After 90 minutes it is filtered off and washed twice with 50 ml. of dry ether. 

This method has been applied successfully to the preparation of phenoxybenzene-4,4 -dithiol (84% of the theoretical amount), diphenylmethane-4,4 -dithiol, and m-sulfhydrylbenzoic acid4 (80%). It did not prove satisfactory for the preparation of higher-melting thiols of lower solubility, such as 2,7-naphtha-lenedithiol, 2,6-naphthalenedithiol, and 4,4 -biphenyldithiol. These were better prepared by the use of tin (II) chloride 2-hydrate in glacial acetic acid saturated with hydrogen chloride.6... 

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