[특허]Synthesis of amine boranes and polyhedral boranes

THE CURATORS OF THE UNIVERSITY OF MISSOURI

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Synthesis of amine boranes and polyhedral boranes

특허상세정보
국가/구분	United States(US) Patent 등록
국제특허분류(IPC7판)	C07F-005/02 C07F-005/05
출원번호	US-0116375 (2015-02-03)
등록번호	US-10179795 (2019-01-15)
국제출원번호	PCT/US2015/014234 (2015-02-03)
국제공개번호	WO2015/117123 (2015-08-06)
발명자 / 주소	Safronov, Alexander Valentinovich Jalisatgi, Satish Subray Hawthorne, Marion Frederick
출원인 / 주소	THE CURATORS OF THE UNIVERSITY OF MISSOURI
대리인 / 주소	Stinson Leonard Street LLP
인용정보	피인용 횟수 : 0 인용 특허 : 5

초록

The present invention relates in general to a method for the synthesis and purification of 1) the polyhedral borane decahydrodecaborate and dodecahydrododecaborate anions and their salts and 2) amines and amine boranes. The organoammonium halide is combined with alkali metal tetrahydroborate to form organoammonium tetrahydroborate, which upon pyrolysis provides organoammonium decahydrodecaborate and organoammonium dodecahydrododecaborate.

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1. A method for synthesizing mixtures of salts of polyhedral boranes, comprising: combining a methyltriethylammonium halide with an alkali metal tetrahydroborate in a reaction mixture;reacting the methyltriethylammonium halide and the alkali metal tetrahydroborate to form a methyltriethylammonium tetrahydroborate intermediate and an alkali metal halide; andpyrolyzing the methyltriethylammonium tetrahydroborate intermediate to produce a product mixture comprising methyltriethylammonium decahydrodecaborate and methyltriethylammonium dodecahydrododecaborate. 2. The method of claim 1, wherein the reacting step and the pyrolizing step are performed as a continuous heating step; and wherein the pyrolizing step comprises pyrolizing the methyltriethylammonium tetrahydroborate intermediate in situ in the reaction mixture. 3. The method of claim 1, further comprising: prior to the reacting step, adding to the reaction mixture a polar aprotic solvent; andprior to the pyrolizing step, separating the methyltriethylammonium tetrahydroborate intermediate from the reaction mixture. 4. The method of claim 3, wherein the polar aprotic solvent is selected from the group consisting of dimethylformamide, dimethylacetamide, dimethylsulfoxide, sulfolane, and hexamethylphosphoramide. 5. The method of claim 3, wherein the intermediate separating step comprises: filtering the reaction mixture to produce a filtrate comprising the methyltriethylammonium tetrahydroborate intermediate; andprecipitating the methyltriethylammonium tetrahydroborate intermediate from the filtrate with a second solvent. 6. The method of claim 1, wherein the pyrolizing step is conducted at a temperature between 180° C. and 200° C. for between 1 and 4 hours. 7. The method of claim 1, wherein the methyltriethylammonium halide is selected from the group consisting of methyltriethylammonium chloride and methyltriethylammonium bromide. 8. The method of claim 1, wherein the alkali metal tetrahydroborate is selected from the group consisting of sodium tetrahydroborate and potassium tetrahydroborate. 9. The method of claim 5, wherein the second solvent is a linear or cyclic ether. 10. The method of claim 9, wherein the linear or cyclic ether is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,4-dioxane, and dimethoxyethane. 11. The method of claim 1, further comprising separating the methyltriethylammonium decahydrodecaborate and the methyltriethylammonium dodecahydrododecaborate in the product mixture based on water solubility. 12. The method of claim 11, wherein said product mixture contains the alkali metal halide and said product mixture separating step comprises: combining the product mixture with cold water to produce a product mixture solution;filtering the product mixture solution to produce a filter cake comprising methyltriethylammonium dodecahydrododecaborate and a product mixture filtrate comprising methyltriethylammonium decahydrodecaborate, methyltriethylammonium dodecahydrododecaborate and the alkali metal halide. 13. The method of claim 12, further comprising the step of purifying the methyltriethylammonium dodecahydrododecaborate from the filter cake. 14. The method of claim 13, wherein the purifying step comprises dissolving the filter cake in acetonitrile and recrystallizing the methyltriethylammonium dodecahydrododecaborate from the acetonitrile to produce a crystalline residue comprising the methyltriethylammonium dodecahydrododecaborate. 15. The method of claim 12, further comprising removing methyltriethylammonium dodecahydrododecaborate from the product mixture filtrate. 16. The method of claim 15, wherein the removing step comprises evaporating the water in the product mixture filtrate to form a residue comprising the methyltriethylammonium decahydrodecaborate;re-dissolving the residue in additional water to produce a methyltriethylammonium decahydrodecaborate solution;filtering the methyltriethylammonium decahydrodecaborate solution to form a second filtrate comprising the methyltriethylammonium decahydrodecaborate, wherein decahydrodecaborate is present as a dianion; andprecipitating the decahydrodecaborate dianion from the second filtrate. 17. The method of claim 16, wherein the precipitating step comprises adding to the second filtrate a halide selected from the group consisting of trialkylammonium halides, tetraalkylammonium halides and tetraalkylphosphonium halides. 18. The method of claim 17, wherein the halide is an ammonium halide selected from the group consisting of tetrabutylammonium bromide, tetrabutylammonium chloride, tributylammonium chloride, and tributylammonium bromide. 19. The method of claim 15, wherein the removing step comprises evaporating the water in the product mixture filtrate to form a residue comprising the methyltriethylammonium decahydrodecaborate;re-dissolving the residue in additional water to produce a methyltriethylammonium decahydrodecaborate solution;filtering the methyltriethylammonium decahydrodecaborate solution to form a second filtrate comprising the methyltriethylammonium decahydrodecaborate wherein decahydrodecaborate is present as a dianion; andisolating the decahydrodecaborate dianion using an ion exchange resin. 20. The method of claim 3, wherein said methyltriethylammonium decahydrodecaborate and said methyltriethylammonium dodecahydrododecaborate in said product mixture are separated based on water solubility, and wherein said product mixture separating step comprises: combining the product mixture with cold water to produce a product mixture solution;filtering the product mixture solution to produce a filter cake comprising methyltriethylammonium dodecahydrododecaborate and a product mixture filtrate comprising methyltriethylammonium decahydrodecaborate wherein decahydrodecaborate is present as a dianion. 21. The method of claim 20, further comprising the step of purifying the methyltriethylammonium dodecahydrododecaborate from the filter cake. 22. The method of claim 21, wherein the purifying step comprises dissolving the filter cake in acetonitrile and recrystallizing the methyltriethylammonium dodecahydrododecaborate from the acetonitrile to produce a crystalline residue comprising the methyltriethylammonium dodecahydrododecaborate. 23. The method of claim 20, wherein the product mixture separating step further comprises precipitating the decahydrodecaborate dianion from the product mixture filtrate. 24. The method of claim 23, wherein the decahydrodecaborate dianion precipitating step comprises adding to the product mixture filtrate a halide selected from the group consisting of trialkylammounium halides, tetraalkylammonium halides and tetraalkylphosphonium halides. 25. The method of claim 24, wherein the halide is an ammonium halide selected from the group consisting of tetrabutylammonium bromide, tetrabutylammonium chloride, tributylammonium chloride, and tributylammonium bromide. 26. The method of claim 20, wherein the product mixture separating step further comprises isolating the decahydrodecaborate dianion using an ion exchange resin. 27. The method of claim 1, wherein the pyrolizing step is conducted in a reactor attached to a two-stage condensation system, wherein a first stage condenser collects a mixture of methyldiethylamine borane, triethylamine borane, methyldiethylamine, and triethylamine, and a second stage condenser collects a mixture of methyldiethylamine and triethylamine. 28. The method of claim 27, wherein said mixture of methyldiethylamine borane, triethylamine borane, methyldiethylamine, and triethylamine is collected and distilled by fractional distillation to separate the methyl di ethyl amine borane, triethylamine borane, methyldiethylamine, and triethylamine. 29. The method of claim 27, wherein the mixture of methyldiethylamine and triethylamine is collected and distilled by fractional distillation to separate the methyldiethylamine and triethylamine. 30. The method of claim 1, wherein the alkali metal tetrahydroborate is 10B-enriched alkali metal tetrahydroborate. 31. The method of claim 30, wherein the 10B-enriched alkali metal tetrahydroborate is synthesized by: first, reacting 10B-enriched boric acid with a C2-C4 alcohol in a reaction mixture that does not include toluene, xylene, mesitylene, benzene, or 1,2-dichlorhoethane to produce trialkylborate-10B;second, reacting the trialkylborate-10B with a metal aluminum hydride in the presence of an amine to produce amine borane-10B; andthird, reacting the amine borane-10B with a reagent selected from the group consisting of alkali metal hydride and alkali metal methoxide to produce alkali metal tetrahydroborate-10B. 32. A method for synthesizing mixtures of salts of polyhedral boranes, comprising: combining a methyltriethylammonium halide with an alkali metal tetrahydroborate in a reaction mixture; andpyrolizing the reaction mixture to produce a product mixture comprising methyltriethylammonium decahydrodecaborate, methyltriethylammonium dodecahydrododecaborate and an alkali metal halide. 33. A method for synthesizing mixtures of salts of polyhedral boranes, comprising: combining a methyltriethylammonium halide, an alkali metal tetrahydroborate and a solvent selected from the group consisting of dimethylformamide, dimethylacetamide, dimethylsulfoxide, and sulfolane, hexamethylphosphoramide to form a methyltriethylammonium tetrahydroborate intermediate and an alkali metal halide;separating the methyltriethylammonium tetrahydroborate intermediate from the reaction mixture; andpyrolizing the methyltriethylammonium tetrahydroborate intermediate to produce a product mixture comprising methyltriethylammonium decahydrodecaborate and methyltriethylammonium dodecahydrododecaborate. 34. A method for separating a methyltriethylammonium decahydrodecaborate and a methyltriethylammonium dodecahydrododecaborate from a mixture based on water solubility wherein the separating step comprises: combining the mixture with cold water to produce a mixture solution; andfiltering the mixture solution to produce a filter cake comprising methyltriethylammonium dodecahydrododecaborate and a product mixture filtrate comprising methyltriethylammonium decahydrodecaborate.

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