Granular lithium

Tri-if-butyltinlithium, (n-C4H9)3SnLi (1), 8, 495-497 10, 413-414 11, 551-552. The reagent can be prepared by reaction of ( -C4H9)3SnCl with excess granular lithium in THF. 

Granular lithium chloride from Mallinckrodt, Inc. was stored in a dry box prior to use. The checkers stored the LiCI in a desiccator before use. 

To a boiling tetrahydrofuran solution (100 mL) of 3.7c (3.0 g, 8.2 mmol) and fert-butyl alcohol (6.2 g, 83.6 mmol) was added granular lithium (0.7 g, 100.9 mmol) in small portions with vigorous stirring over 1 h, and heating was continued for additional 12 h. The mixture was poured into ice water (300 mL) and extracted with petroleum ether. The... 

Mixtures of granular lithium with perhalogenated carbon compounds such as poly-chlorotrifluoroethylene, (ClFCCF2)n, (PCTFE), are reported to yield low combustion temperatures when reacted in confinement (constant volume). The measured combustion temperatures are given below in Table 8.7. Thermochemical codes fail to converge for these fuel-rich stoichiometries as the reaction products are in the condensed phase exclusively. 

Lithium. Several processes for lithium [7439-93-2], Li, metal production have been developed. The Downs cell with LiCl—KCl electrolyte produces lithium ia much the same manner as sodium is produced. Lithium metal or lithium—aluminum alloy can be produced from a mixture of fused chloride salts (108). Granular Li metal has been produced electrochemically from lithium salts ia organic solvents (109) (see LiTHlUM AND LITHIUM compounds). 

Koshina et al. have reported that there are three kinds of morphology [40] dendritic, granular and mossy. Mossy lithium is formed when the deposition current is small and the salt concentration is high. This mossy lithium provides a high cycling efficiency. 

Figure 2. (a) Schematic description for the growth of dendrite crystals on a Li surface. The film consisting of decomposition products as shown in Scheme 1 prevents the growth of large granular crystals but rather promotes the formation of treelike dendrites, (b) Schematic description for the formation of isolated lithium particles from Li dendrites. The uneven dissolution of the dendrites leaves lithium crystals detached from the lithium substrate. The isolated lithium crystals become electrochemically dead but chemically reactive due to their high surface area. 

If the reduction has been carried out in ether, the ether layer is separated after the acidification with dilute hydrochloric or sulfuric acid. Sometimes, especially when not very pure lithium aluminum hydride has been used, a gray voluminous emulsion is formed between the organic and aqueous layers. Suction filtration of this emulsion over a fairly large Buchner funnel is often helpful. In other instances, especially in the reductions of amides and nitriles when amines are the products, decomposition with alkalis is in order. With certain amounts of sodium hydroxide of proper concentration a granular by-product - sodium aluminate - may be separated without problems [121],... 

It is found that lithium can be plated with virtually 100% efficiency in a range of organic systems however, the plated lithium cannot be stripped quantitatively, especially if the cell has been allowed to stand for a period between plating and stripping. An explanation for this behaviour, advanced by Brummer of EIC Corporation, is illustrated in Fig. 7.5. The lithium is considered to be electrode posited in granular form and the newly created surfaces react rapidly with components of the electrolyte this continues... 

SYNTHESIS A solution was made of 12.1 gN,N,N ,N -tetramethylethylenediamine and 13.8 g of 1,3-dimethoxybenzene in 200 mL 30-60 °C petroleum ether. This was stirred vigorously under a He atmosphere and cooled to 0 °C with an external ice bath. There was added 66 mL of 1.6 M butyl lithium in hexane which produced a white granular precipitate. Thereaction mixture was brought up to room temperature for a few minutes, and then cooled again to 0 °C. There was then added 18.7 g of... 

Reaction Mixtures. Wear butyl rubber gloves, laboratory coat, and eye protection. In the fume hood behind a shield, cautiously and slowly carry out the following procedure. Treat the stirred reaction mixture from n grams of lithium aluminum hydride by successive dropwise addition of n mL of H20, n mL of 15% sodium hydroxide solution and 3n mL of H20. This produces a granular precipitate that is removed by filtration and treated as normal refuse. Wash the filtrate into drain.17... 

To a suspension of 117 g of lithium aluminum hydride in 2 L of anhydrous ether (under an inert atmosphere) is added dropwise a solution of 428 g of methyl 2-(pyrrol-l-yl)benzoate in 1.5 L of ether over a period of 4 hours. The reaction mixture is then heated at reflux temperature for an additional 4 hours and then allowed to cool to room temperature. After cooling in an ice-bath, the excess lithium aluminum hydride is destroyed by the dropwise addition of 117 ml of water over 1 hour, followed by dropwise addition of 117 ml of 15% sodium hydroxide and subsequent addition of 351 ml of water over a 30 minute period. The resultant granular solid is separated by filtration, the ether layer is then dried over magnesium sulfate and the solvent evaporated under reduced pressure to yield 2-(pyrrol-l-yl)benzyl alcohol which may be further purified by distillation in vacuum BP 110°-114°C/0.1 mm Hg. 

Lithium trihydridozincate( 1 —) is a white, granular solid which slowly turns black on standing at room temperature. If it is stored at Dry Ice temperature, it remains white for an indefinite period of time. It is not soluble to any extent in ethereal solvents, and it is very sensitive to air and moisture. It is best identified by its x-ray powder diffraction (nickel-filtered CuKa) pattern. The predominant interplanar spacing and the corresponding relative intensities (estimated visually) are d = 6.25 A (m) 4.45 A (vs) 4.30 A (m) ... 

The monohydrate of the metasilicate, LiaSiC HjO, is obtained as an almost insoluble, white, granular precipitate by the interaction at 80° to 90° C. of a solution of sodium metasilicate and the equivalent amount of lithium chloride in presence of normal lithium hydroxide. It is also produced by dissolving silicic acid dried below 100° C. in twice the theoretical proportion of twice-normal lithium hydroxide at the ordinary temperature, and subsequently heating the solution to 80° C. A readily soluble modification has also been prepared.1... 

During workup of a reduction a voluminous, gelatinous precipitate of hydroxides often makes separation of the product difficult, and attempted solution of the precipitate with excess acid or base leads to large volumes and to emulsions. Steinhardt states that these difficulties can be avoided by following a procedure in which the stirred reduction mixture from n grams of lithium aluminum hydride is treated by successive dropwise addition of n ml. of water, n ml. of 15% sodium hydroxide solution, and 3n ml. of water. This produces a dry granular precipitate which is easy to filter and wash. 

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