反应详情

To 105 mg (0.58 mmol) of the amine from step 3 dissolved in 10 mL DMF was added 175 mg (0.58 mmol) of 1-(2-methoxyethyl)piperidin-4-yl]benzoic acid (this acid was prepared according to the procedure described in PCT Int. Appl. WO 01/58886), 110 mg (0.58 mmol) of EDCI, 78 mg (0.58 mmol) of HOBT and 0.22 mL (2.02 mmol) of N-methylmorpholine. The reaction mixture was stirred at room temperature overnight, partitioned between ethyl acetate and water, dried over magnesium sulfate and concentrated. Column chromatography, eluting with 10% methanol in dichloromethane provided 27.8 mg of the title compound N-((1S,2R)-2-{[(cyanomethyl)amino]carbonyl}cyclohexyl)-4-[1-(2-methoxyethyl)piperidin-4-yl]benzamide.

1. customwas prepared
2. custompartitioned between ethyl acetate and water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated
5. washColumn chromatography, eluting with 10% methanol in dichloromethane