초록 ▼

A method is described for synthesizing decaborane wherein at least about 90% of the boron atoms in the decaborane are the .sup.10 B isotope, comprising the steps of: (a) reacting boric acid with a C.sub.1 to C.sub.10 alkanol to form a .sup.10 B-alkyl borate wherein at least about 90% of the boron at

A method is described for synthesizing decaborane wherein at least about 90% of the boron atoms in the decaborane are the .sup.10 B isotope, comprising the steps of: (a) reacting boric acid with a C.sub.1 to C.sub.10 alkanol to form a .sup.10 B-alkyl borate wherein at least about 90% of the boron atoms in the boric acid are the .sup.10 B isotope; (b) reducing the .sup.10 B-alkyl borate to form an alkali metal .sup.10 B-borohydride; (c) converting the alkali metal .sup.10 B-borohydride to a .sup.10 B-tetradecahydroundecaborate ion; and (d) converting the .sup.10 B-tetradecahydroundecaborate ion to .sup.10 B-decaborane. Methods of preparing tetradecahydroundecaborate ions and decaborane from alkali metal borohydrides are also described.

대표청구항 ▼

[ We claim:] [1.] A method for preparing a tetradecahydroundecaborate ion comprising contacting in an inert, non-aqueous solvent medium and at a temperature of from about 85.degree. C. to about 135.degree. C.:(a) a tetrahydroborate having the formulaEQU MBH.sub.4 rein M represents an ion selected fr

[ We claim:] [1.] A method for preparing a tetradecahydroundecaborate ion comprising contacting in an inert, non-aqueous solvent medium and at a temperature of from about 85.degree. C. to about 135.degree. C.:(a) a tetrahydroborate having the formulaEQU MBH.sub.4 rein M represents an ion selected from the group consisting of sodium, potassium, lithium, cesium, rubidium, and lower alkyl ammonium;(b) an alkyl halide of the formulaEQU RX rein R represents an alkyl group of from 1 to about 10 carbon atoms and X represents chloride, bromide, or iodide; and(c) a catalyst selected from the group consisting of iodine, alkali metal iodides, ammonium iodide, bromine, alkali metal bromides, ammonium bromide, and mixtures thereof;with the proviso that an additional amount of said catalyst is added to said inert, non-aqueous solvent medium over and above any of said catalyst that is formed in situ during said contacting process. [24.] A method for preparing a tetradecahydroundecaborate ion comprising:(a) suspending in an inert, non-aqueous solvent medium and at a temperature of from about 85.degree. C. to about 135.degree. C. a tetrahydroborate having the formulaEQU MBH.sub.4 rein M represents an ion selected from the group consisting of sodium, potassium, lithium, cesium, rubidium, and lower alkyl ammonium forming a suspension;(b) adding to said suspension(i) an alkyl halide of the formulaEQU RX rein R represents an alkyl group of from 1 to about 10 carbon atoms and X represents chloride, bromide, or iodide; and(ii) a catalyst selected from the group consisting of iodine, alkali metal iodides, ammonium iodide, bromine, alkali metal bromides, ammonium bromide, and mixtures thereof,such that said tetrahydroborate, said alkyl halide, and said catalyst come into contact thereby forming a tetradecahydroundecaborate ion.