Preparation of carboranyl sulfides

Claim 1

A process for preparation of carboranylmethyl alkyl sulfides comprising: (a) combining a predetermined amount of decaborane with a predetermined amount of cyclohexane to form a mixture in a suitable reaction container that is provided with means for heating, means for cooling, and means for stirring, said container being equipped with a condenser and means for venting of gaseous reaction products; (b) stirring said decaborane and cyclohexane until most of the decaborane is dissolved; (c) adding a predetermined amount, including an excess of the theoretical amount, of a propargyl alkyl sufide to said mixture, said propargyl alkyl sulfide having the formula: HC.tbd.CCH 2 SR, where R equals an alkyl group having from 2 to 10 carbon atoms; (d) refluxing said mixture having said propargyl alkyl sulfide added thereto at a predetermined temperature range and for a predetermined period of time while reacting is accomplished and venting of gaseous reaction products, including hydrogen, is accomplished, said reacting forming a crude reaction product in solution; (e) cooling said crude reaction product in solution; (f) transferring said crude reaction product in solution to a suitable container for separating said crude reaction product; (g) washing said crude reaction product in solution a plurality of times with a 10% potassium hydroxide solution and followed by washing a plurality of times with a solution selected from water and saline solution to thereby effect separating of said crude reaction product that has been washed; (h) transferring the separated and washed crude reaction product in solution to a distillation assembly; (i) distilling the volatile materials, including any excess propargyl alkyl sulfide, until a temperature of about 110° C. is reached, and thereafter, continue distilling the remaining volatiles while gradually reducing the pressure to about 1 mm and while gradually reducing the temperature to about 100° C.; and (j) separating the reaction product by further distilling at a reduced pressure of about 0.5 mm and at a temperature from about 110° C. to about 160° C., said reaction product being a carboranylmethyl alkyl sulfide having the structure: ##STR5## where R equals an alkyl group having from 2 to 10 carbon atoms.