Preparation of lithium aluminum hydride
According to Wiberg (Z. Naturforsch. 7b, 59, 1952), the preparation of lithium aluminum hydride is more easy performed with aluminum bromide compared to aluminum chloride.
To 750 ml of very pure and dry ether, in the small portion 267 g aluminium bromide are added and the mixture is cooled with ice-salt mixture. 33 grams (or 4.1 moles) of coarsely ground lithium hydride is added to the tree-necked flask with a reflux condenser, a stirrer and a dropping funnel. 250 ml of ether are slowly added to cover lithium hydride and aluminum bromide solution is slowly started to run in. The addition of aluminum bromide takes one to two hours. Then the reaction mixture is refluxed for few hours. The lithium bromide and unreacted lithium hydride precipitate on cooling which are decanted through a layer of glass wool. Meanwhile, the filtrate obtained consists of an ether solution of lithium aluminium hydride saturated with lithium bromide. The solution may be stabilized by storing it over a small quantity of lithium hydride.
Handbook of preparative inorganic chemistry, by G. Brauer, Vol 1, 1963, 805-807.
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