反应详情

In a 250 mL three-necked flask under N2 atomosphere, to a solution of 7.2 g of 4-ethoxy-but-3-en-2-one (63 mmol, 1 eq) and 12.7 g of TEA (126 mmol, 2 eq) in THF at −78° C., was added 21 g of TMSOTf (95 mmol, 1.5 eq) dropwise in 40 mins. Stirring was continued for 60 mins at 0˜−30° C. After the conversion was complete (check by NMR), the reaction was quenched with 5% NaHCO3, extract with Hexane and dried over Na2SO4. After remove the solvent the crude product was purified with redistillation (oil pump, <<1 mmbar: Bp, 40° C., Toluene; Bp, 115° C., product) to give 9.1 g pure product. Yield: 72.2%.

1. customthe reaction was quenched with 5% NaHCO3
2. extractionextract with Hexane
3. dry with materialdried over Na2SO4
4. customAfter remove the solvent the crude product
5. distillationwas purified with redistillation (oil pump, <<1 mmbar: Bp, 40° C., Toluene; Bp, 115° C., product)