Methods of synthesis of isotopically enriched borohydride and methods of synthesis of isotopically enriched boranes
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C01B-006/15
C01B-006/17
C01B-006/19
C01B-006/21
C01B-006/23
C01B-035/18
출원번호
UP-0047165
(2005-01-28)
등록번호
US-7641879
(2010-02-11)
발명자
/ 주소
Spielvogel, Bernard
Cook, Kevin
출원인 / 주소
SemEquip Inc.
대리인 / 주소
Edwards Angell Palmer & Dodge LLP
인용정보
피인용 횟수 :
14인용 특허 :
8
초록▼
The invention provides new methods for the synthesis of isotopically enriched metal borohydrides, metal tetrahydroundecaborate salts, and decaborane from isotopically enriched 10B-boric acid or 11B-boric acid. The invention is particularly useful for synthesis of isotopically enriched sodium or lith
The invention provides new methods for the synthesis of isotopically enriched metal borohydrides, metal tetrahydroundecaborate salts, and decaborane from isotopically enriched 10B-boric acid or 11B-boric acid. The invention is particularly useful for synthesis of isotopically enriched sodium or lithium borohydride, MB11H14 (where M is Li, Na, K, or alkylammonium), and decaborane.
대표청구항▼
What is claimed is: 1. A method of synthesizing an isotopically enriched metal borohydride, the method comprising the steps of: (a) providing isotopically enriched boric acid; (b) contacting the isotopically enriched boric acid with an alcohol under conditions conducive to formation of an isotopica
What is claimed is: 1. A method of synthesizing an isotopically enriched metal borohydride, the method comprising the steps of: (a) providing isotopically enriched boric acid; (b) contacting the isotopically enriched boric acid with an alcohol under conditions conducive to formation of an isotopically enriched borate; and (c) reducing the isotopically enriched borate with a metal aluminum hydride under conditions conducive to formation of isotopically enriched metal borohydride. 2. The method of claim 1, wherein the isotopically enriched borate is a compound of Formula I: [(RO)2B—O—]n—R′ wherein each occurrence of R is independently selected from the group consisting of linear or branched alkyl, cycloalkyl, cycloalkyl-alkyl, alkenyl, aryl, aralkyl, haloalkyl, and alkylether, or two R groups taken in combination form α,ω-alkylene group or a 1,2-cylcoalkylene group each of which may be optionally substituted with one or more groups selected from the group consisting of alkyl, alkenyl, cycloalkyl, cycloalkyl-alkyl, aryl, aralkyl, and alkoxy; n is 1 or 2; and R′ is selected from the group consisting of alkyl, alkenyl, aryl, aralkyl, haloalkyl, and alkylether when n=1, or R′ is a α,ω-alkylene group or a 1,2-cylcoalkylene group each of which may be optionally substituted with one or more groups selected from the group consisting of alkyl, alkenyl, cycloalkyl, cycloalkyl-alkyl, aryl, aralkyl, and alkoxy when n=2. 3. The method of claim 1, wherein the isotopically enriched borate is a compound of the formula, B(OR)3, wherein R is independently selected at each occurrence from the group consisting of linear or branched C1-10alkyl , phenyl, benzyl, C3-8cycloalkyl, C3-8cycloalkyl-C1-10alkyl, C2-10alkenyl, C1-10alkoxy, C1-10haloalkyl, and C2-10alkylether. 4. The method of claim 3, wherein the isotopically enriched borate is a compound of the formula, B(OR)3, wherein each occurrence of R is the same and R is selected from the group consisting of linear or branched C1-10alkyl, phenyl, benzyl, C3-8cycloalkyl, C3-8cycloalkyl-C1-10alkyl, C2-10alkenyl, C1-10alkoxy, C1-10haloalkyl, and C2-10alkylether. 5. The method of claim 1, wherein the isotopically enriched borate is a compound of Formula II: wherein R2 and R3 are independently selected at each occurrence from the group consisting of hydrogen, linear or branched alkyl, cycloalkyl, cycloalkyl-alkyl, alkenyl, aryl, aralkyl, haloalkyl, and alkylether; and p is an integer selected from 1-5. 6. The method of claim 5, wherein the isotopically enriched borate is a compound of the formula: wherein q is 1 or 2; and Rx, Rx, and Ry are independently selected at each occurrence from the group consisting of hydrogen, linear and branched C1-10alkyl, C1-10alkoxy, and C3-8cycloalkyl, or Rx and Ry, taken in combination form a α,ω-alkylene group. 7. The method of claim 6, wherein Rx and Ry are selected from the group consisting of hydrogen and linear or branched C1-4alkyl. 8. The method of claim 1, wherein esterification step comprises contacting isotopically enriched boric acid with at least three equivalents of a linear or branched C1-10alkanol or at least one and a half (1.5) equivalents of a C2-10alkanediol. 9. The method of claim 8, wherein the esterification step comprises contacting the isotopically enriched boric acid with at least three equivalents of a linear C2-10alkanol or at least one and a half (1.5) equivalents of a linear or branched 1,2-C2-10alkanediol. 10. The method of claim 9, wherein the esterification step comprises contacting the isotopically enriched boric acid with about three equivalents of a linear C2-10alkanol or about one and a half (1.5) equivalents of a linear or branched 1,2-C2-10alkanediol. 11. The method of claim 1, wherein water generated during the esterification step is removed from the reaction mixture. 12. The method of claim 1, wherein the water is removed from the reaction mixture by distillation. 13. The method of claim 12, wherein the water is removed as an azeotrope with a member selected from the group consisting of toluene, xylene, benzene, 1,2-dichloroethane, and mixtures thereof. 14. The method of claim 1, wherein the esterification step is conducted at a temperature of above about 80° C. 15. The method of claim 1, wherein the esterification step is conducted at a temperature of between about 95° C. and about 175° C. 16. The method of claim 1, wherein the reduction step comprises contacting the borate with a mixture of a metal aluminum hydride and at least one solvent. 17. The method of claim 16, wherein at least one solvent is selected from the group consisting of diethyl ether, tetrahydrofuran, 1,3-dioxolane, 1,4-dioxane, 1,3-dioxane, methyl-tert-butyl ether, dimethoxyethane, diglyme, and mixtures thereof. 18. The method of claim 17, wherein the mixture comprises at least one additional hydrocarbon solvent selected from the group consisting ofbenzene, cyclohexane, methylcyclohexane, toluene, xylenes, linear and branched C5-10alkanes, petroleum ethers, and mixtures thereof. 19. The method of claim 1, wherein the metal aluminum hydride is selected from the group consisting of Group I and Group II metal Aluminum hydrides, and mixtures thereof. 20. The method of claim 19, wherein the metal aluminum hydride is lithium aluminum hydride or sodium aluminum hydride. 21. A method of preparing isotopically enriched metal tetradecahydroundecaborate salt, the method comprising the steps of: (a) providing isotopically enriched metal borohydride by carrying out the method of claim 1; and (b) contacting a solution of the isotopically enriched metal borohydride with a compound of the formula, R—X or isotopically enriched BY3(ligand), under conditions conducive to the formation of a metal tetradecahydroundecaborate salt, wherein R is alkyl, alkenyl, or aralkyl; X is fluoro, chloro, bromo, iodo, alkylsulfonate, or arylsulfonate; Y is fluoro, chloro, or bromo; and the ligand of BY3(ligand) is absent, an ether, an amine, or a pyridine. 22. The method of claim 21, wherein the metal borohydride and the compound of the formula, R—X are contacted at a temperature of between about 50° C. and about 200° C. or wherein the metal borohydride and the isotopically enriched compound of the formula, BY3(ligand) are contacted at a temperature of between about 50° C. and about 200° C.
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