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Bull. Soc. Fr. 1965, 1007-1014 discloses the use of phosphoric acid. 3-Methyl-2-butenal is stirred with ethanol, triethyl orthoformate and phosphoric acid at room temperature for 40 hours. The reaction mixture is then taken up in ether, washed with 0.5 N aqueous ammonia and dried over sodium sulfate. Subsequent distillation affords 3-methyl-2-butenal diethyl acetal in a yield of 65%.

1. washwashed with 0.5 N aqueous ammonia
2. dry with materialdried over sodium sulfate
3. distillationSubsequent distillation