反应详情

温度

60 °C

A mixture of 610 mg (1.8 mmol) 1-[(3S,4S)-1-Benzyl-3-(4-chloro-phenyl)-piperidin-4-yl]-ethylamine, 1.18 g (2.8 mmol) 2-bromo-5-cyano-pyridine and 0.838 g (2.8 mmol) DIPEA in 3.5 mL DMF was heated to 60° C. for 3 days. The mixture was evaporated, Na2CO3aq. was added and the mixture was extracted with ethyl acetate. The combined organic phases were dried with Na2SO4 and evaporated to dryness. The residue was purified by column chromatography on silica eluting with a gradient formed from DCM, methanol and NH3aq. to yield after evaporation of the product containing fractions 0.526 g (66%) of the title compound as off-white foam. MS (m/e): 431.4 [(M+H)+].

1. customThe mixture was evaporated
2. additionwas added
3. extractionthe mixture was extracted with ethyl acetate
4. dry with materialThe combined organic phases were dried with Na2SO4
5. customevaporated to dryness
6. customThe residue was purified by column chromatography on silica eluting with a gradient
7. customformed from DCM, methanol and NH3aq
8. customto yield
9. customafter evaporation of the product
10. additioncontaining fractions 0.526 g (66%) of the title compound as off-white foam