METHOD FOR PRODUCING DECABORANE Russian patent published in 2017 - IPC C01B35/18 

FIELD: chemistry.

SUBSTANCE: invention relates to chemical industry and may be used synthesis and production of unsubstituted and substituted carboranes of a general formula of RCB₁₀H₁₀CR. First a solution of diglyme and sodium borane is heated up to 105°C, while dropwise adding an alkyl halide. After all alkyl halide is added, the reaction mass is stirred for 60 minutes at the same temperature. The resulting product is cooled down to a room temperature under nitrogen gas flow. Diglyme and unreacted alkyl halide distilled off at a residual pressure of 10-15 mm Hg and temperature of 60-90°C to achieve a solid residue. A hydrocarbon solvent is added to the resulting solid product and stirred, 40% aqueous sulphuric acid is added dropwise at a room temperature. The reaction mix is then kept at 50°C until it stops producing gas. The resulting acidic solution of sodium diglymate undecaborate is cooled down to 35°C. An oxidising agent comprising organic compounds with carbonyl groups (aldehydes and ketones) are added dropwise for 15-185 min. The oxidation reaction takes place in the presence of sodium halide, resulting from the condensation reaction. When oxidising agent is added, stirring is stopped and the reaction mass is left to rest until phase separation, the bottom aqueous phase is removed, and the top organic phase is washed with distilled water; the hydrocarbon solvent is distilled off until decaborane B₁₀H₁₄ concentration is 17-20%.

EFFECT: increased decaborane yield by 15-25%, simplified sodium undecaborate oxidation stage, reduced process time, reduced process waste.

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