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    Production of alkali metal borohydrides
    7.
    发明授权
    Production of alkali metal borohydrides 失效
    生产碱金属硼氢化物

    公开(公告)号：US3215491A

    公开(公告)日：1965-11-02

    申请号：US5436760

    申请日：1960-09-07

    Applicant: BAYER AG

    Inventor： FRIEDRICH SCHUBERT ,  KONRAD LANG

    IPC: C01B6/00 ,  C07F5/00

    CPC classification number: C07F5/006 ,  C01B6/00

    Abstract: Alkali metal borohydrides are produced by reacting an alkali metal hydride with a boron trihalide or an addition compound thereof in the presence of an amino borane catalyst of the formula RnB(NR1R11)3-n where R is hydrogen or an alkyl or an aryl radical, R1 is hydrogen or an aliphatic or aryl radical, R11 is an aliphatic or aryl radical, n is an integer from 0 to 2, and the catalyst is present in amounts of from 0,5 to 50% by weight of the alkali metal hydride. The process is carried out in a high boiling (above 180 DEG C.) inert suspension agent such as aliphatic and aromatic hydrocarbons, or inert oils such as tetra alkyl silanes, ethers, and polyethers, and at a temperature between 30 DEG C. and the decomposition temperature of the alkali metal borohydride formed. The boron trihalide addition compounds may be those with di lower alkyl ethers, cyclic alkyl ethers, tri-lower alkyl amines, tertiary mixed lower alkyl aryl amines and pyridine, or it may be Na2O.4BF3. The catalyst may be produced in situ by reacting an amine (R1R11NH) with an N-alkyl borazane selected from pyridine borane, N-tri-lower alkyl borazanes and N-di-lower alkyl borazanes; or R1R11NH with an alkali metal borohydride and a boron halide compound; or R1R11NH with a hydrocarbon substituted diborane of the formula (RnBH3-n)2 where n = 1 or 2. A co-catalyst may be added to the reaction mixture, which is a tertiary alkyl or aryl amine or an alkyl ether capable of forming addition compounds with boron trihalides. The co-catalyst may be present in amounts of 0,5 to 50% by weight of the alkali metal hydride. Examples are given in which boron trifluoride-tetrahydrofuranate is reacted with sodium hydride in the presence of (C3H7)2BN(C4H9)2, acid trisanilide, boric acid trisanilide with a cocatalyst triethylamine, N-triethylborazane with a co-catalyst dibutylamine. Numerous examples of R, R1 and R11 and also of the boron trihalide addition compounds are given.ALSO:Amino boranes of formula RnB(NR1R11)3,n where R represents hydrogen, alkyl or aryl group, R1 represents hydrogen, aliphatic or aryl group, R11 represents an aliphatic or aryl radical, n is 0, 1 or 2 are produced by reacting an amine R1R11NH with an N-alkyl borazane selected from pyridine borane, N-tri C1-C4 alkyl borazanes, N-di-C1-C4 alkyl borazanes. Alternatively the amine R1R11NH may be reacted with a mixture of alkali metal borohydride and boron trihalide or addition compound thereof, or it may be reacted with a hydrocarbon substituted diborane (RnBH3-n)2 where n=1 or 2.

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