110-03-2

white crystalline flakes

The raw materials (37.4 g, 263 mmol), ethyl acetate (60 mL), and Pd/C catalyst (0.285 g, 2.63 mmol, 1 mol %) were added to an autoclave. The hydrogen gas was slowly added until10 bar. When the hydrogenation reaction was performed for 12 hours and then the hydrogen gas was removed. Finally, 2,5-Dimethyl-2,5-hexanediol is obtained by purification.

Synthesis, p. 165, 1981 DOI: 10.1055/s-1981-29377

Purify the diol by fractional crystallisation. Then the diol is dissolved in hot acetone, treated with activated charcoal, and filtered while hot. The solution is cooled and the diol is filtered off and washed well with cold acetone. The crystallisation process ia repeated several times, and the crystals are dried under a vacuum in a freeze-drying apparatus [Goates et al. J Chem Soc, Faraday Trans 1 78 3045 1982]. [Beilstein 1 IV 2600.]

[1] Feghouli G, et al. Activation of reducing agents. Sodium hydride containing complex reducing agents 29. Epimerization of alcohols by nickel-containing complex reducing agents (NiCRA). Tetrahedron Letters, 1988; 9: 285–290.