O=[CH:2][C:3](=C)[CH3:4].C(O)C.C(O[CH:12]([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])C>C1(C)C=CC(S(O)(=O)=O)=CC=1.C([O-])([O-])=O.[K+].[K+].C(Cl)Cl>[CH2:17]([O:16][CH:12]([O:13][CH2:14][CH3:15])[C:3](=[CH2:2])[CH3:4])[CH3:18]p-Toluenesulfonic acid (1.14 g, 0.006 mol) was added to a mixture of methacrolein (42.35 g, 0.06 mol), ethanol (141.9 mL), CH2Cl2 (120 mL) and triethylorthoformate (130.6 mL, 0.785 mol). The mixture was stirred at room temperature for 3 days and then K2CO3 (2 g) was added. The mixture was stirred for 10 minutes, filtered, and then the filtrate was concentrated in vacuo. The residue was purified by distillation through a Vigreaux column at 130° C. to afford 35 g of methacrolein diethylacetal.
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