FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing anhydrous nickel (II) acetylacetonate, which is used as a reaction catalyst in synthesis of nitrogen-containing heterocyclic systems, as well as in organic synthesis for producing organometallic compounds. Proposed method includes a step for producing nickel acetylacetonate dihydrate by adding sodium hydroxide to an aqueous solution of nickel sulphate heptahydrate with intense stirring and temperature 15-25 °C with subsequent addition of acetylacetone at temperature of 15-25 °C. Reagents are used at molar ratio of nickel sulphate heptahydrate : sodium hydroxide : acetylacetone, equal to 1:2-2.5:2. Further, nickel acetylacetonate dihydrate crystals are obtained when heating nickel acetylacetonate dihydrate at temperature of 85-90 °C for 1-1.5 hours. Crystals of anhydrous nickel acetylacetonate are obtained by azeotropic distillation of a solution of nickel acetylacetonate dihydrate in toluene with concentration of 20-25 wt.%, followed by filtration of the obtained mother solution and crystallisation of the precipitate while distilling excess toluene from the mother solution. Further, mother solution with precipitated precipitate is cooled to temperature of 10-15 °C followed by holding for 6-8 hours at said temperature and filtering the precipitate.
EFFECT: high output of nickel acetylacetonate.
1 cl, 2 tbl, 3 ex
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Authors
Dates
2024-11-21—Published
2024-04-01—Filed