反应详情

温度

0 °C

A solution of ethylmalonamate (23.6 g, 0.18 mol) in absolute ethanol (300 mL) is added to a stirred solution of diethyl ethoxymethyleneoxalacetate (44.0 g, 0.18 mol) in ethanol (200 mL) at 0° C., followed by the addition, of solid sodium acetate (14.72 g, 0.18 mol). After stirring for ten minutes at 0° C., the mixture is heated to reflux and stirred for 13.5 hours. After cooling, the ethanol is removed under vacuum, and the residue diluted with water and acidified to pH 2 with concentrated hydrochloric acid. The aqueous solution is extracted with methylene chloride (2×200 mL) and the organic layer washed with 300 mL saturated sodium chloride, then dried over anhydrous magnesium sulfate and concentrated in vacuum to give 45.0 g of the title product as an orange oil.

1. temperaturethe mixture is heated
2. temperatureto reflux
3. stirringstirred for 13.5 hours
4. temperatureAfter cooling
5. customthe ethanol is removed under vacuum
6. additionthe residue diluted with water
7. extractionThe aqueous solution is extracted with methylene chloride (2×200 mL)
8. washthe organic layer washed with 300 mL saturated sodium chloride
9. dry with materialdried over anhydrous magnesium sulfate
10. concentrationconcentrated in vacuum