反应详情

温度

0 °C

3-(2,4,5-Trifluorophenyl)propionic acid (3.25 g, 16.0 mmol; from Step 1) was dissolved in THF (15 mL) and cooled to 0° C. To this solution was added Me2S.BH3 (3.2 mL, ˜32 mmol) dropwise under 30 min and the resulting mixture was then heated at 70° C. for 30 min. After cooling to 0° C., 6 M aqueous HCl (20 mL) was added dropwise. The mixture was heated at 70° C. for 1 h. After cooling to room temperature the mixture was extracted with ether (2×20 mL) and the combined organic layers were washed with brine and dried over Na2SO4. Evaporation and drying in vacuum gave the title compound as a colorless liquid (3.17 g, 97% pure by HPLC) that was used directly in the next step. *Previously reported in EP 369812.

1. temperaturethe resulting mixture was then heated at 70° C. for 30 min
2. temperatureAfter cooling to 0° C.
3. temperatureThe mixture was heated at 70° C. for 1 h
4. temperatureAfter cooling to room temperature the mixture
5. extractionwas extracted with ether (2×20 mL)
6. washthe combined organic layers were washed with brine
7. dry with materialdried over Na2SO4
8. customEvaporation
9. customdrying in vacuum