The present invention is directed to a process for the synthesis of alkali metal tetrahydroborates-10B and amine borane-10B precursors, such as sodium tetrahydroborate-10B and triethylamine borane-10B.
대표청구항▼
1. A process for the synthesis of alkali metal tetrahydroborates comprising the following steps: 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,
1. A process for the synthesis of alkali metal tetrahydroborates comprising the following steps: 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. 2. The process of claim 1, wherein the second reacting step utilizes a linear or cyclic ether solvent. 3. The process of claim 2, wherein the linear or cyclic ether solvent is selected from the group consisting of diethyl ether, tetrahydrofuran (THF), 1,4-dioxane, dimethoxyethane (DME), diglyme. 4. The process of claim 1, wherein the third reacting step utilizes a linear or cyclic alkane solvent. 5. The process of claim 4, wherein the linear or cyclic alkane solvent is selected from the group consisting of decalin, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane. 6. The process of claim 1, wherein the C2-C4 alcohol selected from the group consisting of 1-butanol, ethanol, 2-propanol, and 2-butanol. 7. The process of claim 1, wherein the alkali metal is selected from the group consisting of lithium, sodium, potassium and cesium. 8. The process of claim 1, wherein the amine is selected from the group consisting of a tertiary amine, a pyridine or a dialkylaniline. 9. The process of claim 1, wherein the metal aluminum hydride is selected from the group consisting of lithium aluminum hydride, sodium aluminum hydride, and potassium aluminum hydride. 10. The process of claim 2, wherein the second reacting step comprises: forming a mixture of said amine, said metal aluminum hydride, and said solvent;cooling the mixture;adding said trialkylborate-10B dropwise to said mixture to form a second mixture; andallowing said second mixture to warm to room temperature. 11. The process of claim 1, wherein the second reacting step produces a solution comprising said amine borane-10B and said amine borane-10B is separated from the precipitate by filtration. 12. The process of claim 2, wherein excess solvent from said second reacting step is separated from the solution and reused in said second reacting step by distillation. 13. The process of claim 1, wherein the third reacting step produces a suspension comprising said alkali metal tetrahyroborate-10B and said alkali metal tetrahydroborate-10B is separated from the suspension by filtration. 14. The process of claim 4, wherein excess solvent from said third reacting step is separated from the solution by distillation and reused in said third reacting step. 15. The process of claim 1, wherein after said first reacting step excess alcohol is separated from the reaction mixture by distillation and reused in said first reacting step. 16. The process of claim 1, wherein said third reacting step produces amine, the amine is separated from the reaction mixture by distillation, and the amine is reused in said second reacting step. 17. The process of claim 1, wherein said third reacting step produces trimethylborate-10B, the trimethylborate-10B is separated from the reaction mixture by distillation, and the trimethylborate-10B is reused in said second reacting step. 18. The process of claim 1, wherein said third reacting step produces trimethylborate-10B and amine, the trimethylborate-10B and amine are separated from said reaction mixture by distillation during the third reaction step to form a distillate comprising the trimethylborate-10B and amine, and the trimethylborate-10B is separated from amine in the distillate by further distillation. 19. The process of claim 9, wherein the metal aluminum hydride is lithium aluminum hydride and the C2-C4 alcohol is 1-butanol. 20. A process for the synthesis of an amine borane-10B comprising the step of reacting trialkylborate-10B with a metal aluminum hydride in the presence of an amine selected from the group consisting of a tertiary amine, a pyridine or a dialkylaniline. 21. The process of claim 20 wherein the metal aluminum hydride is selected from the group consisting of lithium aluminum hydride, sodium aluminum hydride, or potassium aluminum hydride. 22. The process of claim 20, wherein the trialkylborate-10B is selected from the group consisting of tributylborate-10B and trimethylborate-10B. 23. The process of claim 20, wherein the amine is triethylamine. 24. The process of claim 20, wherein the metal aluminum hydride is lithium aluminum hydride and the C2-C4 alcohol is 1-butanol. 25. A process for the synthesis of alkali metal tetrahydroborate-10B comprising the step of reacting amine borane-10B with a reagent selected from the group consisting of alkali metal hydride and alkali metal methoxide. 26. The process of claim 25, wherein the amine borane-10B is triethylamine borane-10B. 27. The process of claim 25, further comprising adding a linear or acyclic alkane solvent.
연구과제 타임라인
LOADING...
LOADING...
LOADING...
LOADING...
LOADING...
이 특허에 인용된 특허 (5)
Patek Gary (Katy TX), Borohydrides to inhibit polymer formation in petrochemical caustic scrubbers.
Cowan Robert L. ; Ginosar Daniel M. ; Dunks Gary B., Method of synthesizing enriched decaborane for use in generating boron neutron capture therapy pharmaceuticals.
※ AI-Helper는 부적절한 답변을 할 수 있습니다.