At the present time there is a widespread interest in the chemistry of boron. Especially is this true in the field of organo-boron compounds, for boron has been found to possess the property of forming ring and chain compounds with itself or with certain organic groups. Many organo—boron compounds may be prepared by standard organic reactions. Interest has developed in the possible electrochemical formation of boron-containing organic compounds. A considerable saving in materials of construction, power, and reaction time may result if these syntheses are performed electrochemically. The formation of organo-boron compounds may be accomplished through the anodic formation of a free alkyl radical by electrolyzing a solution of an alkyl alkali compound such as lithium ethyl, along with a simultaneous electrolysis of an alkali borohydride. The deposition of the free alkyl radical in the presence of the borohydride radical may result in a reaction between the two. The purpose of this investigation was to study the electrolysis of diethyl ether solutions of lithium methyl, lithium ethyl, lithium butyl, or ethyl magnesium bromide in the presence of lithium borohydride. / Master of Science