A large-scale preparative method for potassium di-n-butylborate
in triethylamine solvent has been developed. The reaction of
potassium di-n-butylborate I with trifluoromethyl iodide has been
shown to yield trifluoromethyl di-n-butylborane and other products.
Reaction of this substance with boron trifluoride gave trifluoromethyl
boron difluoride. Reactions of diboron tetrafluoride, boron tribromide,
and di-n-butylboron chloride with trifluoromethyl mercury
iodide and bis(trifluoromethyl) mercury have also been studied. In
each case a free radical mechanism leads to extensive decomposition
of the trifluoromethyl group.
The design and operation of an all-glass, excepting the stainless
steel detector unit, gas chromatograph is given. The instrument
was operative on both a preparative and analytical scale handling samples that range in size from less than 0.25 ml up to five ml.
The experimental equipment and technique for the determination
of the infrared spectrum of volatile compounds and compounds of marginal
stability is described. The apparatus and technique were used
to determine the infrared spectrum of diboron tetrafluoride
