反应详情

Diethyl 2,2-bis(hydroxymethyl)malonate (20 g, 90.82 mmol), acetone (20 ml), 2,2-dimethoxypropane (20 ml), and concentrated sulfuric acid (0.2 ml) were stirred at 25° C. for 2 days. The reaction was slowly poured into saturated aqueous sodium carbonate. The organic supernatant was separated and concentrated in vacuo. The residue was then dissolved in ether, rinsed with saturated aqueous sodium carbonate and brine, and then dried over magnesium sulfate, filtered and concentrated in vacuo to afford crude 2,2-dimethyl-[1,3]dioxane-5,5-dicarboxylic acid diethyl ester (21.4 g, 91%) as a light yellow oil: 1H NMR (300 MHz, CDCl3) δ ppm 1.27 (t, J=7.1 Hz, 6H, 2×CH3), 1.42 (s, 6H, 2×CH3), 4.24 (q, J=7.1 Hz, 4H, 2×OCH2), 4.29 (s, 4H, 2×OCH2).

1. customThe organic supernatant was separated
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was then dissolved in ether
4. washrinsed with saturated aqueous sodium carbonate and brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo