Diethylaluminium hydride is prepared by reacting triethylaluminium with hydrogen and an aluminium alloy at elevated temperature and superatmospheric pressure, said alloy comprising a major proportion of aluminium and a minor proportion of one or more of the metals titanium, vanadium, zirconium and niobium. It is preferred that the proportion of aluminium should be at least 98% by weight. The reaction is carried out at a temperature between 80 and 200 DEG C. at a pressure between 60 and 350 atmospheres. An excess of hydrogen is used.
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