in dichloromethane BCl3 condensing under N2 at -196°C onto phosphonium salt in CH2Cl2, warming to room temp., stirring for 2 h, cooling to -78°C, volatiles fractionating, diborane collecting at -196°C; identified by IR spectrum;

in dichloromethane BBr3 condensing under N2 at -196°C onto phosphonium salt in CH2Cl2, warming to room temp., stirring for 2 h, cooling to -78°C, volatiles fractionating, diborane collecting at -196°C; identified by IR spectrum;

in dichloromethane byproducts: (CH3P(C6H5)3)HBF3; BF3 condensing under N2 at -196°C onto phosphonium salt in CH2Cl2, warming to room temp., stirring for 2 h, cooling to -78°C, volatiles fractionating, diborane collecting at -196°C; identified by IR spectrum;