反应详情

温度

120 °C

To a solution of methyl 3-oxopentanoate (3 g, 23.1 mmol) in toluene (30 mL) was added ethane-1,2-diol (3 mL, 70.2 mmol) and p-toluenesulfonic acid (500 mg, 2.91 mmol), the resulting mixture was stirred at 120° C. overnight. Then the mixture was concentrated and partitioned between ethyl acetate and aqueous saturated sodium bicarbonate solution. The phases were separated and the aqueous layer was extracted with ethyl acetate. The combined organic phase was washed with brine and dried over sodium sulfate; then it was filtered and concentrated to give methyl 2-(2-ethyl-1,3-dioxolan-2-yl)acetate (1.7 g, 42.5%) as yellow oil which was used without purification. Product tlc [petroleum ether/ethyl acetate (15:1) developed with iodine, Rf 0.6]

1. concentrationThen the mixture was concentrated
2. custompartitioned between ethyl acetate and aqueous saturated sodium bicarbonate solution
3. customThe phases were separated
4. extractionthe aqueous layer was extracted with ethyl acetate
5. washThe combined organic phase was washed with brine
6. dry with materialdried over sodium sulfate
7. filtrationthen it was filtered
8. concentrationconcentrated