METHOD OF PRODUCING CRYSTALLINE LITHIUM-ALUMINUM DEUTERIDE Russian patent published in 2019 - IPC C01B6/24 C01B4/00 C01D15/00 C01F7/00 

FIELD: technological processes.

SUBSTANCE: invention relates to production of metal deuterides for use as a selective reducing agent in organic synthesis, for deuteration of medicinal preparations for further use in medicine and pharmaceutics. Method of producing crystalline lithium aluminum deuteride LiAlD₄ includes reaction of lithium deuteride with aluminum chloride in medium of diethyl ether in temperature range of 10÷15 °C while stirring with disperser at 3,500 rpm for 30÷60 min. Obtained clarified solution is decanted and toluene is added thereto in volume ratio of diethyl ether to toluene of 1.5–1.33:1. Crystallisation is carried out by distilling diethyl ether and heating to 90÷92 °C. Precipitated residue of crystalline lithium aluminum deuteride is dried under vacuum at 60 °C for 2 hours. Aluminum chloride solution is preliminarily prepared by dissolving AlCl₃ in diethyl ether while cooling to temperature of 0…-5 °C.

EFFECT: invention enables to obtain pure coarse-crystalline lithium aluminum deuteride, increases its output, and reduces explosion and explosion hazard of the process.

1 cl, 3 ex