反应详情

温度

55 °C

Step 1 A stirred suspension of tert-butyl ethyl malonate (2.01 mL, 10.6 mmol), 1,2-dibromoethane (1.01 mL, 11.7 mmol), potassium carbonate (3.67 g, 26.6 mmol) and 1-butyl-3-methylimidazolium tetrafluoroborate (0.198 mL, 1.06 mmol) in DMF (26.6 mL) was heated to 55° C. for 20 hours. Upon cooling the mixture was filtered and the solid residue was washed with Et2O. The mixture was diluted with Et2O and washed with water (×2). The organic phase was dried (Na2SO4), filtered and concentrated giving 1-tert-butyl 1-ethyl cyclopropane-1,1-dicarboxylate which was used without further purification, 2.24 g.

1. temperatureUpon cooling the mixture
2. filtrationwas filtered
3. washthe solid residue was washed with Et2O
4. additionThe mixture was diluted with Et2O
5. washwashed with water (×2)
6. dry with materialThe organic phase was dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated