Isolated salt hydrates

Thorium compounds of anionic nitrogen-donating species such as [Th(NR2)4], where R = alkyl or sdyl, are weU-known. The nuclearity is highly dependent on the steric requirements of R. Amides are extremely reactive, readily undergoing protonation to form amines or insertion reactions with CO2, COS, CS2, and CSe2 to form carbamates. Tetravalent thorium thiocyanates have been isolated as hydrated species, eg, Th(NCS)4(H20)4 [17837-16-0] or as complex salts, eg, M4 Th(NCS)g] vvH20, where M = NH, Rb, or Cs. 

Ghromium(II) Compounds. The Cr(II) salts of nonoxidizing mineral acids are prepared by the dissolution of pure electrolytic chromium metal ia a deoxygenated solution of the acid. It is also possible to prepare the simple hydrated salts by reduction of oxygen-free, aqueous Cr(III) solutions using Zn or Zn amalgam, or electrolyticaHy (2,7,12). These methods yield a solution of the blue Cr(H2 0)g cation. The isolated salts are hydrates that are isomorphous with and compounds. Examples are chromous sulfate heptahydrate [7789-05-17, CrSO 7H20, chromous chloride hexahydrate... 

Lithium chloride, LiCl.—The anhydrous salt is obtained by evaporating to dryness in a current of hydrogen chloride or in presence of ammonium chloride the solution formed by dissolving the carbonate in hydrochloric acid, or decomposing the sulphate with barium chloride.4 Bogorodsky 5 has isolated three hydrates at very low temperatures the trihydrate, LiCl,3H20, is deposited in small needles at —15° C. the dihydrate, LiCl,2H20, crystallizes in cubes and at 12-5° C. octa-hedra of the monohydrate, LiCl,H20, are formed. At about 98° C. the anhydrous salt separates. 

N-Isopropylhydroxylamine and 5-formylfuran-2-sulfonic acid, sodium salt hydrate (5.94 g), were refluxed in 200ml methyl alcohol 24 hours. Thereafter, another portion of N-isopropylhydroxylamine was added and the mixture refluxed 24 hours, then solvent was removed and a yellow solid isolated. The solid was re-crystallized in EtOAc and the product isolated in 15% yield, mp = 230 °C (dec). and C-NMR and IR data supplied. 

It was only in 1995 that the first structure of a hydrated salt of scandium containing only water molecules in its coordination sphere was reported. Refluxing scandium oxide with triflic acid leads to the isolation of hydrated scandium triflate Sc(03SCF3)3 9H20. It is isomorphous with the hydrated lanthanide triflates, containing tricapped trigonally prismatic coordinate scandium in the [Sc(H20)g] ions, with Sc—O (vertices) = 2.171(9) A and Sc—O (face capped) 2.47(2) A. 

The hexafluorophosphate ion has proved to be very useful for studies with complexes, since the [PF6] anion has a very weak coordinating ability.1 Lan-thanoid hexafluorophosphates can be obtained in very concentrated aqueous solutions by reaction of a freshly prepared solutions of hexafluorophosphoric acid and a hydrated lanthanoid basic carbonate.2 The resulting solution, after filtration, is evaporated to near dryness. Attempts to isolate the hydrated salts are unsuccessful because of decomposition accompanied by hydrogen fluoride evolution. Nevertheless, the complexes containing diphenylphosphinic amide are isolable and are quite stable.3... 

Because of the highly electrophilic nature of the 1,2-oxazinium cation, virtually no studies have been carried out on isolated salts no general chemistry has been developed comparable to that of the pyrylium salts. There are, however, some reports of reactions in which 1,2-oxazinium salts are likely to be transient intermediates. Early work on 3,5,6-triaryl-l,2-oxazinium cations indicated that on hydration they are converted into the corresponding 6-hydroxy-6//-oxazinium cations (Equation... 

Zinc nitrate can be obtained as one of several hydrates, of which Zn(N03)2-6H20 is the most common. Anhydrous Zn(N03)2 is made from Zn and N2O4 since heating the hydrates yields hydroxy salts. The hexahydrates of Zn(N03)2 and Zn(C104)2 contain octahedral [Zn(OH2)e] in the solid state. Similarly, it is possible to isolate salts containing [Zn(NH3)6] from reactions done in liquid NH3, e.g. ZnCl2-6NH3. However, in aqueous solution,... 

Whilst in Bordeaux, Laurent isolated pimaric acid from pine tar. From coal tar he isolated phenol (hydrate de phenyle ou acide phenisique) and obtained picric acid by nitrating it. He proved that phenol is identical with the carbolic acid (karbolsaure) discovered in coal tar by Runge. Laurent described the preparation of purer specimens of chlorophenols and showed that the chlorindoptic acid prepared by Erdmann from indigo is pentachloro-phenol. Laurent prepared trinitrophenol (acide nitrophenisique) and its salts and showed that it is identical with the substance discovered by Woulfe (see Vol. Ill, p. 301) and named picric acid (acide picrique) by Dumas (m/cpo , bitter), who translated as acide carbazotique Liebig s name kohlenstickstoff-saure. The chrysoleptic acid obtained by the action of nitric acid on aloes by Schunck he himself found was picric acid. 

The actinide ions in aqueous solution resemble the tripositive lanthanide ions in their precipitation reactions, allowing for differences in the redox properties of early members of the actinide series. The chloride, bromide, nitrate, bromate, and perchlorate anions form water-soluble salts, which can be isolated as hydrated solids by evaporation. The acetates, iodates, and iodides are somewhat less soluble in water. The sulfates are sparingly soluble in hot solutions, somewhat more soluble in the cold. Insoluble precipitates are formed with hydroxide, fluoride, carbonate, oxalate, and phosphate anions. Precipitates formed from aqueous solution are usually hydrated, and the preparation of anhydrous salts from the hydrates without formation of hydrolyzed species can only be accomplished with difficulty. The actinide(iv) ions resemble Ce(iv) in forming fluorides and oxalates insoluble even in acid solution. The nitrates, sulfates, perchlorates, and sulfides are all water-soluble. The iv state actinide ions form insoluble iodates and arsenates even in rather strong acid solution. The... 

Iron(III) hydroxide [1309-33-7], FeH02, is a red-brown amorphous material that forms when a strong base is added to a solution of an iron(III) salt. It is also known as hydrated iron(III) oxide. The fully hydrated Fe(OH)3 has not been isolated. The density of the material varies between 3.4-3.9 g/cm, depending on its extent of hydration. It is insoluble in water and alcohol, but redissolves in acid. Iron(III) hydroxide loses water to form Fe203. Iron(III) hydroxide is used as an absorbent in chemical processes, as a pigment, and in abrasives. Salt-free iron(III) hydroxide can be obtained by hydrolysis of iron(III) alkoxides. 

BeryUium chloride [7787-47-5], BeCl2, is prepared by heating a mixture of beryUium oxide and carbon in chloride at 600—800°C. At pressures of 2.7—6.7 Pa (0.02—0.05 mm Hg) beryllium chloride sublimes at 350—380°C. It is easily hydrolyzed by water vapor or in aqueous solutions. BeryUium chloride hydrate [14871-75-1] has been obtained by concentrating a saturated aqueous solution of the chloride in a stream of hydrogen chloride. ChloroberyUate compounds have not been isolated from aqueous solutions, but they have been isolated from anhydrous fused salt mixtures. 

Bismuth trioxide may be prepared by the following methods (/) the oxidation of bismuth metal by oxygen at temperatures between 750 and 800°C (2) the thermal decomposition of compounds such as the basic carbonate, the carbonate, or the nitrate (700—800°C) (J) precipitation of hydrated bismuth trioxide upon addition of an alkah metal hydroxide to a solution of a bismuth salt and removal of the water by ignition. The gelatinous precipitate initially formed becomes crystalline on standing it has been represented by the formula Bi(OH)2 and called bismuth hydroxide [10361 -43-0]. However, no definite compound has been isolated. 

EDA reacts readily with two moles of CS2 in aqueous sodium hydroxide to form the bis sodium dithiocarbamate. When aqueous ammonia and 2inc oxide (or manganese oxide or its hydrate) is used with a basic catalyst, the 2inc (or manganese) dithiocarbamate salt is isolated. Alternatively, the disodium salt can react with ZnSO or MnSO followed by dehydration in an organic solvent to yield the same salts (48—50). 

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