α,α,α',α'-Tetramethyltetramethylene glycol (CAS NO.: ), which is also known as , 2,5-dimethyl-, could be produced through the following synthetic routes.

Tertiary butyl alcohol (900 ml., 702 g., 9.47 moles) is dissolved in a solution prepared by mixing 28 ml. (0.50 mole) of concentrated sulfuric acid with 1.5 l. of water in a 5-l. round-bottomed flask equipped with a thermometer, stirrer, gas inlet tube, and two addition burets. One buret is charged with 86 ml. (1 mole) of 11.6M hydrogen peroxide, and the other with a solution of 278 g. (1 mole) of ferrous sulfate pentahydrate and 55.5 ml. (1 mole) of concentrated sulfuric acid in 570 ml. of water. The reaction flask is swept out with nitrogen and cooled to 10° by means of an ice bath. Stirring is commenced and the two solutions are added simultaneously and equivalently over a period of 20 minutes. The temperature is held below 20°.

When the addition is completed, 50 ml. (1 mole) of 52% sodium hydroxide is added with stirring and cooling, and then 450 g. of anhydrous sodium sulfate (not all of the salt dissolves). The cold solution is transferred to a separatory funnel and the phases are separated. The organic layer is neutralized with 52% sodium hydroxide; approximately 20 ml. is required to bring the pH to 7. The aqueous layer, including the precipitated ferric hydroxide, is added to the aqueous portion of the reaction mixture and the whole is extracted with 400 ml. of t-butyl alcohol. This extract is similarly treated with 52% sodium hydroxide (about 5 ml. is required). The resulting aqueous layer is combined with the main aqueous fraction, which is again extracted with 400 ml. of t-butyl alcohol. This whole process is again repeated so that the organic phases comprise the three extracts and the phase which separated initially from the reaction mixture.

The four organic fractions are combined and distilled under reduced pressure. The distillation is continued until the temperature of the flask is about 70°/5 mm. in order to remove most of the t-butyl alcohol. The still residue is then extracted with 2 l. of ether and the extract is treated with decolorizing carbon and diatomaceous earth. Distillation of the ether at slightly reduced pressure from a water bath yields α,α,α',α'-tetramethyltetramethylene glycol as a pale yellow crystalline residue weighing 30–45 g. (41–62% yield based on hydrogen peroxide employed). The crude product is digested at room temperature in a mixture of 30 ml. of ether and 70 ml. of cyclohexane. The resulting slurry is filtered to yield 29–34 g. (40–46%) of the glycol as a white crystalline solid, m.p. 87–88°. The product, which is pure enough for most purposes, can be further purified by recrystallization from ethyl acetate (1 g. in 4 ml.), cyclohexane (1 g. in 20 ml.), or water (1 g. in 2 ml.).