反应详情

温度

-78 °C

At −78° C., 6.0 g (0.0205 mol) of ethyl (4-fluoro-2-trifluoromethylbenzoylamino)acetate dissolved in THF were added dropwise to 24.3 ml (0.049 mol) of a 2M lithium diisopropylamide solution in THF. After 1 h at −78° C., 1.4 g (0.025 mol) of acrolein dissolved in THF were added dropwise, and the mixture was stirred at −78° C. for 1 h. Saturated NH4Cl solution was then added, and the mixture was allowed to warm to RT. The mixture was extracted with CH2Cl2, and the combined organic phases were then washed and dried and the solvent was removed. The residue was purified chromatographically (SiO2; cyclohexane/ethyl acetate). This gave 4.7 g (66% of theory) of the title compound as a colorless solid (diastereomer mixture) which was reacted further without further purification.

1. additionwere added dropwise
2. temperatureto warm to RT
3. extractionThe mixture was extracted with CH2Cl2
4. washthe combined organic phases were then washed
5. customdried
6. customthe solvent was removed
7. customThe residue was purified chromatographically (SiO2; cyclohexane/ethyl acetate)
8. customThis gave 4.7 g (66% of theory) of the title compound as a colorless solid (diastereomer mixture) which was reacted further without further purification