反应详情

To a 500 mL round-bottom flask was added biphenyl-2-ylcarbamic acid piperidin-4-yl ester (17.0 g, 58 mmol) and N-(4-[1,3]dioxolan-2-yl-2,5-dimethylphenyl)acrylamide (13.1 g, 52.9 mmol). Ethanol (150 mL) and dichloromethane (150 mL) were added to form a slurry. The reaction mixture was heated at 50° C. to 55° C. for about 24 hours and then cooled to room temperature. Most of the solvent was removed on a rotary evaporator, resulting in a thick slurry. Ethanol (reagent grade) was added to form a total volume of about 200 mL and the resulting mixture was heated to 80° C. and then cooled slowly to room temperature. The resulting thick white slurry was filtered, washed with ethanol (20 mL) and dried in vacuum to provide biphenyl-2-ylcarbamic acid 1-[2-(4-[1,3]dioxolan-2-yl-2,5-dimethylphenylcarbamoyl)ethyl]piperidin-4-yl ester (23.8 g, about 98% purity) as a white solid.

1. customto form a slurry
2. temperatureThe reaction mixture was heated at 50° C. to 55° C. for about 24 hours
3. customMost of the solvent was removed on a rotary evaporator
4. customresulting in a thick slurry
5. customto form a total volume of about 200 mL
6. temperaturethe resulting mixture was heated to 80° C.
7. temperaturecooled slowly to room temperature
8. filtrationThe resulting thick white slurry was filtered
9. washwashed with ethanol (20 mL)
10. customdried in vacuum