反应详情

温度

80 °C

A mixture of 50 grams (0.27 mole) of diethyl ethylidenemalonate, 455 grams (4.02 moles) of 30% hydrogen peroxide, 17.6 gram (0.053 mole) of sodium tungstate dihydrate and 400 milliliters of ethanol was stirred and heated at 80° C. for one hour, cooled to room temperature and stirred for an additional hour. Ethanol was removed under reduced pressure and the produce extracted into dichloromethane (3×200 milliliters), the extract then water-washed, dried (MgSO4), filtered and solvent removed to give the crude product. Vacuum distillation gave 40.45 grams (0.20 mole) of diethyl 3-methyloxirane-2,2-dicarboxylate having a boiling point of 120° C. at 4millimeters of Hg.

1. temperaturecooled to room temperature
2. stirringstirred for an additional hour
3. customEthanol was removed under reduced pressure
4. extractionthe produce extracted into dichloromethane (3×200 milliliters)
5. extractionthe extract
6. washwater-washed
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customsolvent removed
10. customto give the crude product
11. distillationVacuum distillation