Abstract: A one-step process for preparing 2,5-dimethylhexane-2,5-dihydroperoxide and its alkyl derivatives comprises: (1) adding sulfuric acid to a 60-70% hydrogen peroxide solution to form a first reaction mixture where the first mixture is controlled at a temperature in the range of from about -10.degree. C. to about 10.degree. C.; (2) adding 2,5-dimethyl-2,5-dihydroxy hexane to the mixture held at a temperature in the range of from about -10.degree. C. to about 10.degree. C. or lower to form a second reaction mixture and maintaining the second mixture at a temperature in the range of from about 20.degree. C. to about 50.degree. C. for about 5 minutes to about 5 hours to form a slurry containing the solid product of 2,5-dimethylhexane-2,5-dihydroperoxide, unreacted reactants and impurities; (3) lowering the temperature of the slurry to the range of from about -10.degree. C. to about 10.degree. C.