Patent GB-889599-A (GB)
Title: Process for the production of boron-nitrogen compounds
IPC: C07F5/00
Filed: 1958-09-19
Abstract: Ammonium borohydrides, substituted organically on the N atom, (NR1R11R111R1111)BH\t 4, (where R1, R11, R111, R1111, represent H, aliphatic, cycloaliphatic, or aromatic radicals), or unsubstituted, NH4BH4, or borazanes, substituted organically on the N atom, (NR1R11-R111)BH3, or unsubstituted, NH3BH3, are produced by reacting an alkali (all specified), or alkaline earth, (all specified) metal, NH+4, or Mg. borohydride with an ammonium salt or hydroxide, which has organic substituent radicals on the ammonium N atom, as required, in the presence of liquid NH3, or a liquid amine of formula NRxRxxRxxx (where Rx, Rxx, Rxxx represent H, aliphatic, cycloaliphatic, or aromatic radicals).  Ammonium salts are sulphates, fluorides, chlorides, bromides, iodides, acetates, sulphides or borates of NH+4, NH3CH+3, NH2(CH3)+2, NH(CH3)+3, o N(CH3)+4, corresponding ethyl, propyl, isopropyl, butyl, or isobutyl compounds, C6H5NH+3, C6H5CH3NH+2, C6H5-NH(CH3)+2.  The amine may be mono-, di or tri-, methyl- or ethyl-amine, isopropylamine, propylamine, butylamine, aniline, N-methyl-, -dimethyl-, -ethyl-, or -diethyl-aniline, or cyclohexyldimethylamine.  If the amine is stronger than the base of the ammonium salt or hydroxide, then the salt, or hydroxide, of that base will be formed first, and the borohydride of that base will be produced.  The borohydrides may be isolated by filtering off the precipitated salt and evaporating the amine in vacuo at -10 to 0 DEG C.  If the evaporation is effected at 0-130 DEG C. in some cases, H2 or alkane is liberated and the borazane results.  If the reaction product obtained in liquid NH3 has, e.g. trimethylamine, cyclohexyldimethylamine, or pyridine, added before evaporation, then the borazane of the respective amine is isolated.  Specifications 859,468 and 871,569 are referred to.ALSO:Ammonium borohydrides, substituted organically on the N atom, (NR1R11R111R1111)BH4, (where R1, R11, R111, R1111, represent H, aliphatic, cycloaliphatic, or aromatic radicals), or borazanes, substituted organically on the N atom, (NR1R11R111)BH3, are produced by reacting an alkali (all specified), or alkaline earth (all specified) metal, NH4+, or Mg. borohydride with an ammonium salt or hydroxide, which has organic substituent radicals on the ammonium N atom, as required, in the presence of liquid NH3, or a liquid amine of the formula NRxRxxRxxx (where Rx, Rxx, Rxxx represent H, aliphatic, cycloaliphatic, or aromatic radicals).  Ammonium salts are sulphates, fluorides, chlorides, bromides, iodides, acetates, sulphides or borates of NH3CH3+, NH2(CH3)2+, NH(CH3)3+, or N(CH3)4+, corresponding ethyl, propyl, isopropyl, butyl, or isobutyl compounds, C6H5NH3+ C6H5CH3NH2+ C6H5NH(CH3)2+.  The amine may be mono-, di- or trimethyl- or ethyl-amine, isopropylamine, propylamine, butylamine, aniline, N-methyl-, -dimethyl-, -ethyl-, or -diethylaniline, or cyclohexyldimethylamine.  If the amine is stronger than the base of the ammonium salt or hydroxide, then the salt, or hydroxide, of that base will be formed first, and the borohydride of that base will be produced.  The borohydrides may be isolated by filtering off the precipitated salt and evaporating the amine in vacuo at-10 DEG  to 0 DEG C.  If the evaporation is effected at 0 DEG C.-130 DEG C. in some cases, H2 or alkane is liberated and the borazane results.  If the reaction product obtained in liquid NH3 has, e.g. trimethylamine, cyclohexyldimethylamine, or pyridine, added before evaporation, then the borazane of the respective amine is isolated.  Specifications 859,468 and 871,569 are referred to.