|Institution:||Oregon State University|
|Full text PDF:||http://hdl.handle.net/1957/47858|
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.