in neat (no solvent) BCl3 condensing under N2 at -196°C onto ammonium salt, warming to 0°C, stirring for 1 h, cooling to -196°C, warming slowlyto room temp. while the volatiles pumping off, borane collecting at -140°C; identified by IR spectrum;

in neat (no solvent) BBr3 condensing under N2 at -196°C onto ammonium salt, warming to 0°C, stirring for 1 h, cooling to -196°C, volatiles fractionating, target borane collecting at -140°C, solid residue acidifying, analyzing by NMR spectrum; identified by IR spectrum;

in neat (no solvent) byproducts: (CH3(CH2)3)4NHBF3; BF3 condensing under N2 at -196°C onto ammonium salt, warming to0°C, stirring for 3 h, cooling to -196°C, volatiles fractionating, borane collecting at -140°C; identified by IR spectrum;

HBr in dichloromethane byproducts: H2; HBr condensing onto ammonium borate in CH2Cl2 at -196°C, warmingto -78°C for 1 h, then stirring at room temp.for several minutes, BBr3 and CH2Cl2 condensing at -196°C, stirring at -78°C for 12 h, fractionating; identified by IR and NMR spectra;