Patent GB-956394-A (GB)
Title: Boron compounds and their preparation
Inventor: KNOTH WALTER HENRY
IPC: C01B21/092
Filed: 1961-04-28
Abstract: The invention comprises compounds of the formula Ma(B10H10-yXy)b, where M is an ato or group of atoms which forms a cation, X is a monovalent substituent capable of replacing hydrogen in a benzene nucleus, y is 1-10, and a and b are 1, 2, or 3, the values of a and b being such that a multiplied by the valence of M is equal to 2b.  M may be hydrogen, hydronium (H3O+), ammonium, hydroazonium, or a metal.  The compounds are prepared by reacting a compound of the formula Ma(B10H10)b (made as described in Specifications 956,391, 956,392 and 956,393) with a reagent used for introducing substituents into the benzene nucleus. The substituent X may be halogen, cyano, nitro, nitroso, azo, sulpho, or sulphonyl; nitro compounds may be reduced to amino compounds which may be converted to amido compounds. Examples describe the preparation of the following compounds: CsHB10 HCl7(NO)2, (H3O)2B10CL9NO2 and its caesium salt, Cs2B10HBr7(NO)2, (H3O)2B10H5 (NO2)5, (NH4)2B10Cl5(NO2)5.  By passin corresponding salt solutions through an ion exchange resin, acids are obtained, for example H2B10 HBr7(NO)2 and H2B10Br10.  Alkali metal, alkaline earth metal, and heavy metal salts of the acids may be formed by reaction with a base or a heavy metal salt; compounds formed are Cs2B10Br10 and Ag2B10Br10 whic is useful in photographic processes.ALSO:The invention comprises compounds of the formula Ma (B10H10-yXy)b where M is an atom or group of atoms which forms a cation, X is a monovalent substituent capable of replacing hydrogen in a benzene nucleus, y is 1-10, and a and b are 1, 2, or 3, the values of a and b being such that a multiplied by the valence of M is equal to 2b.  M may be hydrogen, hydronium (H3O+), ammonium, hydrazonium, N-substituted ammonium or hydrazonium, or a metal. The compounds are prepared by reacting a compound of the formula Ma(B10H10)b (made as described in Specifications 956,391, 956,392 and 956,393) with a reagent used for introducing substituents into the benzene nucleus.  The substituent X may be halogen, hydrocarbon, carboxyl, N,N-disubstituted amido, acyl halide, cyano, trihalomethyl, acyl, aldehyde, nitro, nitroso, azo, sulpho, sulphonyl, or mercuric acetyl.  Acyl halide groups may be hydrolyzed to carboxyl and esterified with alcohols; nitro compounds can be reduced to amino compounds and converted to amido compounds. Examples describe the preparation of the following <FORM:0956394/C2/1> [(CH3)4N]2 B10H5Br5 and similar compounds with 7, 9, and 10 bromine atoms, [(C2H5)4N]2B10H6Br4, [(CH3)4N]2B10H6I4, [(CH3)4N]2B10H4BrI5, [(C2H5)4N]2B10H9NO, [(CH3)4N]2B10Cl9NO2 and the corresponding acid and caesium salt, [(CH3)4N]2B10H2Br7NO, [(CH3)4N]2 B10H5 (NO2)5, [(CH3)4N]2B10Cl5(NO2) 5, H2B10H9 SO2C6H4CH3, H2B10H8(COC6H5)2 and its sodium and tetramethyl ammonium salts, a salt having a phenylazo group attached to the decaborate anion, H2B10H8[CH(CH3)2]2. 3H2O and its caesium salt, and H2B10H8(C6H11)2.XH2O and its caesium salt.  By passing solutions of the salts through an ion exchange resin, the free acids are obtained and these may be converted to alkali metal, alkaline earth metal, or heavy metal salts.ALSO:A solution useful for dyeing wool and viscose rayon fibres a red colour is formed by dissolving in ethanol a phenylazo compound which precipitates when an aqueous solution of benzene diazonium chloride is added to an aqueous solution of diammonium decahydrodecarbonate (NH4)2B10H10. Specifications 956,391, 956,392 and 956,393 are referred to.ALSO:Filter paper which has been treated with an aqueous solution of (NH4)2B10Br10 (see Division C1) does not burn freely when touched with a free flame.  Specifications 956,391, 956,392 and 956,393 are referred to.