反应详情

温度

-78 °C

To a −78° C. solution of LDA (192 mmol) in THF (200 mL) was added 3-ethoxy-cyclohex-2-enone (23 mL) dropwise. After stirring for 1 h at −78° C., ethyl cyanoformate (16 mL) was added. The mixture was stirred at −78° C. for 4 h and then was warmed to rt and stirred for 1 h. The mixture was concentrated, diluted with aq. NH4Cl (300 mL), and poured into water. The resulting solids were collected by suction filtration and washed with hexanes followed by water, then was dried and concentrated to provide 17.1 g of a brown solid. TLC (SiO2, 33% EtOAc/hexanes): Rf=0.43.

1. stirringThe mixture was stirred at −78° C. for 4 h
2. temperaturewas warmed to rt
3. stirringstirred for 1 h
4. concentrationThe mixture was concentrated
5. additiondiluted with aq. NH4Cl (300 mL)
6. additionpoured into water
7. filtrationThe resulting solids were collected by suction filtration
8. washwashed with hexanes
9. customwas dried
10. concentrationconcentrated