5694-68-8

71516-48-8

5694-68-8

General procedure for the synthesis of 1,3-dioxane-2-methanol from the compound (CAS: 71516-48-8): (66b) Preparation of 1,3-dioxan-2-ylmethanol: To a solution of 2-((benzyloxy)methyl)-1,3-dioxan-2-ylmethanol (3.01 g, 15.5 mmol) in methanol (100 mL), obtained in the previous step (66a), was Palladium hydroxide (20 wt% Pd (dry basis) carbon, wet (up to 50% water)) (300 mg) was added. The reaction mixture was stirred at room temperature for 15 hours under hydrogen atmosphere. Upon completion of the reaction, the gas in the reaction vessel was displaced with nitrogen, the catalyst was removed by filtration through diatomaceous earth and washed with methanol. The filtrate was concentrated and dried under reduced pressure to afford 1,3-dioxane-2-methanol (1.57 g, 97.3% yield) as a light yellow oil.1H NMR (400 MHz, CDCl3) δ ppm: 1.89 (1H, br s), 3.66-3.72 (2H, m), 3.88-4.08 (4H, m), 5.01 (1H, t, J = 3 Hz).