反应详情

温度

40 °C

A mixture of (2R)-4-(5-bromo-3-trifluoromethyl-pyridin-2-yl)-2-methyl-piperazine-1-carboxylic acid tert-butyl ester from step (c) above (8.48 g, 20 mmol), methyl acrylate (1.9 g, 22 mmol, Aldrich), palladium acetate (49 mg, 2.0 mmol, Aldrich) and benzyltriethyl ammonium chloride (456 mg, 2.0 mmol, Aldrich) in DMF (20 mL) was stirred at 40° C. for 18 h. The reaction mixture was cooled to room temperature, diluted with water (50 mL) and extracted with EtOAc (2×80 mL). The combined organic extracts were washed with brine (40 mL), dried over Na2SO4 and filtered. The filtrate was evaporated in vacuo and the residue was purified by silica gel column chromatography, eluting with 20% EtOAc/hexane to give the title compound as a white solid. MS (ESI, pos. ion) m/e: 430 (M+1).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted with EtOAc (2×80 mL)
3. washThe combined organic extracts were washed with brine (40 mL)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customThe filtrate was evaporated in vacuo
7. customthe residue was purified by silica gel column chromatography
8. washeluting with 20% EtOAc/hexane