This experiment describes a method for cyclohexene oxidation to "trans"-1,2-cyclohexanediol using "p"-toluenesulfonic acid ("p"-TsOH) as promoter and hydrogen peroxide as oxidant in a biphasic system. This method allows conversions up to 97.9% (monitored by [superscript 1]H NMR). "trans"-1,2-Cyclohexanediol was not easily separated from the aqueous solution owing to formation of an azeotropic mixture with water. Destruction of the azeotropic mixture was observed in the presence of sodium "p"-toluenesulfonate salt ("p"-TsONa). Therefore, water could be removed by simple distillation after "p"-TsOH neutralization. Purification of "trans"-1,2-cyclohexanediol was accomplished by sublimation. The overall reaction, separation, and purification experiment did not require any organic solvent. (Contains 1 scheme.)