A desirable solvent replacement has been effected in the synthesis of persubstituted phosphonitrilic hydroquinone prepolymer materials. The replacement of carbon tetrachloride with cyclohexane has no adverse effect on the composition and quality of the material prepared. The overall yield of the reaction increases from 65 to 70% and the toxicity of the reaction mixture and of the waste generated from the reaction are greatly reduced. The particularly close match of solvent properties between carbon tetrachloride and cyclohexane makes this an excellent solvent replacement. Such changes to less-expensive, less-toxic, and less-environmentally damaging solvents are on the increase. A brief list of some known replacement solvents for use in polymer and coatings applications is presented. © 1994 John Wiley & Sons, Inc.