反应详情

温度

60 °C

To a stirred solution of 3-[5-chloro-6-(cyano-dimethyl-methyl)-pyridin-3-yl]-propionic acid ethyl ester (0.68 g, 2.43 mmol) from step 4 above, in 1:1 THF/H2O (4 mL) was added 2 N NaOH (2.43 mL). The resulting solution was stirred at 60° C. for 1 hour. Solvents were removed and residue was partitioned between ethyl acetate and 10% citric acid and extracted. The organic phase was washed with brine (50 mL), dried over Na2SO4 and evaporated. The residue solidified to a white solid and was used without further purification. (0.39 g, 64%) as a white solid. ESIMS (MH−): 251.

1. customSolvents were removed
2. customresidue was partitioned between ethyl acetate and 10% citric acid
3. extractionextracted
4. washThe organic phase was washed with brine (50 mL)
5. dry with materialdried over Na2SO4
6. customevaporated
7. customwas used without further purification