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ChemicalBook CAS DataBase List 1 1-DIETHOXY-3-METHYL-2-BUTENE 97
1740-74-5

1 1-DIETHOXY-3-METHYL-2-BUTENE 97 synthesis

11synthesis methods
-

Yield:1740-74-5 89%

Reaction Conditions:

with Mo11O40PV*4H(1+) in ethanol at 20; for 1 h;Green chemistry;Reagent/catalyst;

Steps:

2.4.2. General procedure for the synthesis of1,1-diethoxy-3-methyl-2-butene

PMo11V was used as catalyst in this preparation. Triethyl orthoformate (18 mmol), 3-methyl-2-butenal (18 mmol), and the catalyst (PMo11V, 1 mmol %) were added to absolute ethanol (5 mL) at 20 °C. The progress of the reaction was monitored by thin layer chromatography (TLC) and gas chromatography (GC) analyses. After stirring for 1 h, the excess of ethanol was removed by evaporation, and the resulting mixture was treated with toluene (10 mL); finally, the catalyst was recovered by centrifugation and washing with toluene (5 mL). The organic phase was dried on anhydrous Na2SO4, filtered and concentrated to obtain the crude acetal. The acetal was isolated as a clear, colorless liquid by vacuum distillation (89% yield, 116-119 °C at 170 mm Hg, and 117.0-118.5 °C at 171-172 mm Hg).

References:

Romanelli, Gustavo;Sathicq, ángel;Vázquez, Patricia;Villa, Aída;Alarcón, Edwin;Grajales, Edwing;Cubillos, Jairo [Journal of Molecular Catalysis A: Chemical,2015,vol. 398,p. 11 - 16]