Patent GB-889600-A (GB)
Title: Process for the production of borazanes
IPC: C07F5/00
Filed: 1959-04-06
Abstract: Borazane, or a borazane having 1, 2, or 3 organic substituents on the N atom, or in which the N atom forms part of a heterocyclic ring is prepared by reacting a complex metal borohydride as claimed in Specification 871,202 with an acid, at below the decomposition temperature of the borazane to be produced, in solution or suspension in water, liquid NH3, a liquid organic amine, or a heterocyclic nitrogen base.  A complex borohydride of the ammonia, amine or base is allegedly formed as an intermediate, in such media, which decomposes to the borazane with evolution of H2.  The solvent or suspension medium is preferably therefore the amine component of the desired borazane, but if the complex metal borohydride contains an amine ligand, which is more strongly basic than the medium, this may form the amine component of the intermediate borohydride.  The borazane will in general contain the least volatile of the amine components present.  H2S is the preferred acid, being added either with the medium, or subsequently to decompose the intermediate borohydride, with precipitation of heavy metal sulphide.  The borazane may be purified by distillation, or by dissolution in ether, shaking with charcoal, and evaporation of the ether.  The example refers to the action of H2S:- on [Cd(NH3)6](BH4)2 suspended in (C2H5)3N or (CH3)2NH to form (C2H5)3N.BH3 or (CH3)2NH.BH3; on [Zn(NH3)4] (BH4)2 suspended in C5 H5 N or (C2H5)3N to form C5 H5 N.BH3 or (C2H5)3N.BH3; or on [Cd(CH3 NH2)6](BH4)2 suspended in (C2H5)3N to form (C2H5)3N.BH3.  Specification 889,599 is referred to.ALSO:A borazane having 1, 2, or 3 organic substituents on the N atom, or in which the N atom forms part of a heterocyclic ring is prepared by reacting a complex metal borohydride as claimed in Specification 871,202 with an acid at below the decomposition temperature of the borazane to be produced in solution or suspension in water, liquid NH3, a liquid organic amine, or a heterocyclic N base.  A complex borohydride of the ammonia, amine, or base is allegedly formed as an intermediate, in such media, which decomposes to the borazane with evolution of H2.  The solvent or suspension medium is preferably, therefore, the amine component of the desired borazane, but if the complex metal borohydride contains an amine ligand, which is more strongly basic than the medium this may form the amine component of the intermediate borohydride.  The borazane will in general contain the least volatile of the amine components present. H2S is the preferred acid, being added either with the medium, or subsequently to decompose the intermediate borohydride, with precipitation of heavy metal sulphide.  The borazane may be purified by distillation, or by dissolution in ether, shaking with charcoal, and evaporation of the ether.  The example refers to the action of H2S on [Cd(NH3)6](BH4)2 suspended in (C2H5)3N or (CH3)2NH to form (C2H5)3N . BH3 or (CH3)2NH . BH3; on [Zn(NH3)4](BH4)2 suspended in C5H5N or (C2H5)3N to form C5H5N.BH3 or (C2H5)3N.BH3; or on [Cd(CH3NH2)6] (BH4)2 suspended in (C2H5)3N to form (C2H5)3N.BH3. Specification 889,599 also is referred to.