反应详情

To a stirred solution of ethyl 3-(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)propanoate (500 mg, 1.6 mmol, step 1 of Example 10) in CH2Cl2 (5 mL), trifluoroacetic acid (1.2 mL, 16 mmol) was added and stirred overnight at room temperature. The mixture was concentrated, and the residual oil was dissolved in CH2Cl2 (60 mL) and solid K2CO3 (5 g) was added, and stirred for 10 min. The mixture was filtered, and the filtrate was concentrated to give ethyl 3-[4-(aminomethyl)piperidin-1-yl]propanoate as a pale yellow oil. Following coupling reaction was carried out according to the procedure described in step 6 of Example 1 from 3,3-dimethyl-1,3-dihydro-2H-indol-2-one (Robertson, David W et al., J. Med. Chem., 1986, 29, 1832) and ethyl 3-[4-(aminomethyl)piperidin-1-yl]propanoate.

1. concentrationThe mixture was concentrated
2. dissolutionthe residual oil was dissolved in CH2Cl2 (60 mL)
3. additionsolid K2CO3 (5 g) was added
4. stirringstirred for 10 min
5. filtrationThe mixture was filtered
6. concentrationthe filtrate was concentrated