Lithium chloride, anhydrous

Lanthanum nitrate, analysis of anhydrous, 5 41 Lead (IV) acetate, 1 47 Lead(II) 0,0 -diethyl dithiophos-phate, 6 142 Lead (IV) oxide, 1 45 Lead(II) thiocyanate, 1 85 Lithium amide, 2 135 Lithium carbonate, formation of, from lithium hydroperoxide 1-hydrate, 5 3 purification of, 1 1 Lithium chloride, anhydrous, 6 154 Lithium hydroperoxide 1-hydrate, 5 1... 

The current primary method for production of lithium is by electrolysis. Spodumene, the most plentiful lithium bearing ore, is beneficiated to 3 to 5% Li20 and heated to 1000°C to convert it from its alpha form to its beta form. The beta form is treated with sulfuric acid to form Li2S04. The Li2S04 is water-soluble and is leached and reacted with sodium carbonate to form lithium carbonate. The lithium carbonate is then reacted with hydrochloric acid to form lithium chloride. Anhydrous lithium chloride is used to produce lithium metal by electrolysis (Austin 1984). 

To a mixture of O.BB mol of anhydrous lithium chloride and 100 ml of OMSO was added a solution of 0.40 mol of the acetylenic tosylate (for a general procedure concerning the preparation of acetylenic tosylates, see Chapter VllI-3, Exp. 3) in IBO ml of DMSO. The flask was equipped for vacuum distillation (see Fig. 5). Between the receiver, which was cooled at -75°C, and the water-pump was placed a tube filled with KOH pellets. The apparatus was evacuated (10-20 mmHg) and the flask gradually heated until DMSO began to reflux in the column. The contents of... 

A solution of 1.0 g of 1,4 (11 )-pregnatriene-170 1 -diol-3 0-dione-21 -acetate and 5,0 g of lithium chloride in 40 ml of glacial acetic acid is treated with 0.410 g of Nchlorosuccinimide, followed by 0.104 g of anhydrous hydrogen chloride dissolved in 2.5 ml of tetrahydrofuran. The reaction mixture is stirred for 2 hours and poured into ice water. The crude product Is filtered and washed with water to give 1.12 g of solid material, which is recrystallized from acetone-hexane to give substantially pure 90 ,11 -dichloro-1,4-pregnadiene-170 ,21 -diol-3,20-dione-21 -acetate MP 246°C to 253°C (dec.). 

C. 4-Methoxy-4 -nitrobiphonyl (3). A dry, 500-mL, three-necked, round-bottomed flask equipped with a reflux condenser, magnetic stirring bar, nitrogen gas inlet, and rubber septum (Note 1) is charged sequentially with 300 mL of anhydrous N,N-dimethylformamide (Note 13), 15.0 g (55.4 mmol) of 4-nitrophenyl trifluoromethanesulfonate (1), 27.8 g (70.0 mmol) of tributyl(4-methoxyphenyl)stannane (2) (Note 14), 7.5 g of dry lithium chloride (Note 15), and 1.6 g (4 mol percent) of bis(triphenylphosphine)palladium(ll) chloride (Note 16). The rubber septum is replaced with a Teflon stopper and the yellow mixture is heated at 100-105°C for 2.5 hr. After approximately 20 min, the reaction turns dark brown. 

A solution of 20.0 g. (0.105 mole) (Note 6) of p-toluenesulfonyl chloride in 100 ml. of anhydrous.ether is then injected into the addition funnel, and this solution is added over a period of 30 minutes to the red reaction mixture at 0° with stirring. The red color immediately disappears upon addition. After addition is complete, 4.2 g. (0.1 mole) of anhydrous lithium chloride (Note 7) is added. The reaction mixture is warmed to room temperature and stirred overnight (18-20 hours), during which time lithium p-toluenesulfonate precipitates. 

Anhydrous lithium chloride purchased from Aldrich Chemical Company, Inc., was used. It is finely pulverized then dried by heating at 200°C (0.1 mm to 0.01 mm) for 6 hr (vacuum oven) before use. The salt is hygroscopic and must be handled very... 

Commercial trimethyl borate contains an appreciable amount of methanol. It is removed by adding anhydrous lithium chloride to the bottle and allowing the mixture to stand with occasional shaking. The upper layer is decanted off and fractionated, b.p. 68-69°. The product must be protected from moisture. 

In an electrolytic cell (Fig. 5) consisting of platinum electrodes (2 cm x 5 cm in area) and cathode and anode compartments separated by an asbestos divider, each compartment is charged with 17 g (0.4 mol) of lithium chloride and 450 ml of anhydrous methylamine. Isopropylbenzene (12 g, 0.1 mol) is placed in the cathode compartment and a total of 50,000 coulombs (2.0 A, 90 V) is passed through the solution in 7 hours. After evaporation of the solvent the mixture is hydrolyzed by the slow addition of water and extracted with ether the ether extracts are dried and evaporated to give 9.0 g (75%) of product boiling at 149-153° and consisting of 89% of a mixture of isomeric isopropylcyclohexenes and 11% of recovered isopropylbenzene. 

The carbon-nitrile bond in cyanoalkanes is cleaved by reduction at very negative potentials. This is the route for decomposition of acetonitrile at tlie limit for its use as an aprotic solvent in electrochemistry [114, 115]. Preparative scale reduction of cyanoalkanes is best carried out in anhydrous ethylamine containing lithium chloride as supporting electrolyte and gives 60-80 % yields of the alkane plus cyanide ion. 

Fig. 23. — The Solubility of Lithium Chloride in Anhydrous and 97 per cent. Pyridine.

B. [ 1 S(R),2S]-N-(2-Hydroxy- 1-methyl-2-phenylethyl)-N,2-dimethylbenzene-propionamide, [(1S,2S)-pseudoephedrine-(R)-2-methylhydrocinnamamide]. A flame-dried, 2-L, three-necked, round-bottomed flask equipped with a mechanical stirrer and an inlet adapter connected to a source of argon is charged with 25.0 g (590 mmol) of anhydrous lithium chloride (Note 6) and sealed with a rubber septum. The inlet adapter is removed and replaced with a rubber septum containing a needle adapter to an argon-filled balloon. The reaction flask is charged with 31.3 mL (223 mmol) of diisopropylamine (Note 7) and 120 mL of tetrahydrofuran (Note 2). The mixture is cooled to -78°C in a dry ice-acetone bath, and 85.1 mL (207 mmol) of a 2.43 M solution of butyllithium in hexanes (Note 8) is added via cannula over 10 min. The resulting suspension is warmed to 0°C in an ice-water bath and is held at that temperature for 5 min, then cooled to -78°C. An ice-cooled solution of 22.0 g (99.4 mmol) of (1 S,2S)-pseudoephedrinepropionamide in 300 mL of tetrahydrofuran (Note 2) is transferred to the cold reaction mixture by cannula over 10 min. The reaction mixture is stirred at -78°C for 1 hr, at 0°C for 15 min, at 23°C for 5 min, and finally is cooled to 0°C, whereupon 17.7 mL (149 mmol) of benzyl bromide (Note 9) is added... 

Anhydrous lithium chloride (99+%, A.C.S. reagent grade) was purchased from Aldrich Chemical Company, Inc., and was further dried as follows. The solid reagent is transferred to a flask fitted with a vacuum adapter. The flask is evacuated (0.5 mm) and immersed in an oil bath at 150°C. After heating for 12 hr at 150°C, the flask is allowed to cool to 23°C and is flushed with argon for storage. 

Lithium Arsenates.—Lithium Orthoarsenate is obtained as the hemihydrate, 2Li3As04.H30, by the action of lithium carbonate on arsenic acid and allowing the solution to crystallise.4 The anhydrous salt is prepared by recrystallising this hydrate from fused lithium chloride 5 rhombic crystals of density 3-07 at 15° C. are obtained. These are soluble in dilute acetic acid they are extremely stable and may be heated to a white heat without fusion. With excess of arsenic acid the normal salt yields deliquescent rhombic prisms of lithium dihydrogen arsenate, 2LiH2As04.3H20, which with water revert to the normal salt.6... 

N,N-Dimethylethanamine, hydrogen chloride (anhydrous, 1.0 M solution in diethyl ether), and lithium tetrahydroaluminate (1 —) are used as purchased from Aldrich. The diethyl ether is distilled from sodium benzo-phenone under nitrogen prior to use. 

Both lyotropic and thermotropic liquid-crystalline synthetic polymers have been widely studied. Aromatic polyamides constitute the most important class forming liquid-crystalline solutions the solvents are either powerfully protonating acids such as 100% sulphuric acid, chloro-, fluoro- or methane-sulphonic acid, and anhydrous hydrogen fluoride, or aprotic dipolar solvents such as dimethyl acetamide containing a small percentage, usually 2-5 %, of a salt such as lithium chloride or calcium chloride. Such solutions constitute a nematic phase within certain limits. Some criteria for formation of a nematic instead of an isotropic phase are ... 

The chloro compound HOCCH(CH3)Cl, b.p. 74 C/760 mmHg, nD(20") 1.4250, can be prepared analogously, using anhydrous lithium chloride. 

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