反应详情

温度

0 °C

A stirred solution of ethyl 3-oxo-3-(2,3,4,5-tetrafluorophenyl)propionate (3.17 g, 12 mmol), acetic anhydride (3.34 mL, 3.6 g, 30 mmol) and triethyl orthoformate (3.00 mL, 2.6 g, 18 mmol) was heated at 130° C. for 1.5 h. The mixture was concentrated in vacuo and dried under high vacuum for 3 hours. The crude product was dissolved in EtOH (15 mL) and cooled to 0° C. and then 1-amino-1-cyclopentanemethanol (1.01 g, 8.8 mmol) was added very slowly. After 1.5 h, the solvent was removed by evaporation to yield the title compound as yellow oil (3.1 g crude) that was used in the next step without further purification.

1. concentrationThe mixture was concentrated in vacuo
2. customdried under high vacuum for 3 hours
3. dissolutionThe crude product was dissolved in EtOH (15 mL)
4. customthe solvent was removed by evaporation