Solubility of sodium aluminum hydride in tetrahydrofuran

Mechanochemical preparation and investigation of properties of magnesium, calcium and lithium–magnesium alanates

“…[17], 1.00 g (9.01 mmol) of CaCl 2 was suspended in 100 ml of THF and stirred for 1 h with a high-speed stirrer. The suspension was then added to a solution of 0.97 g (18.0 mmol) of NaAlH 4 in 200 ml THF and the mixture was stirred for 1 h with a high-speed stirrer.…”

“…Ca(AlH 4 ) 2 ·(THF) x has been earlier prepared from CaH 2 and AlBr 3 or AlCl 3 in dimethyl ether/THF or THF [24][25][26][27] or from CaCl 2 and NaAlH 4 in THF [17]. As found by Dymova and co-workers [9], solvent free Ca(AlH 4 ) 2 , admixed with CaAlH 5 (see below), is formed upon heating or ball milling of CaH 2 /AlCl 3 mixtures (Eq.…”

“…Additionally, following Ref. [17], a nearly pure Ca(AlH 4 ) 2 could be obtained from CaCl 2 and NaAlH 4 in THF and subsequent desolvation of the THF adduct at 60 • C in high vacuum (Eq. (7)).…”

Direct synthesis and NMR characterization of calcium alanate

“…Some solvent always remains within the structure in the as synthesized product and subsequent extraction of the solvent is difficult to achieve without alanate decomposition. A narrow temperature window is generally necessary to purify the compound without decomposition [4,5], making reproducible synthesis difficult. Therefore, a simple and straightforward "dry" method without by product is of great interest because potential candidates for hydrogen storage such as the calcium alanate and other complex hydrides are typically synthesized using solvents.…”

“….) [4][5][6][7][8], the solvent is then removed by moderate heating under vacuum. Mechanochemical synthesis [8] has also been reported using mixtures of NaAlH 4 and CaCl 2 .…”