反应详情

温度

70 °C

To a solution of Methyl 1-[(4-{[(tert-butoxycarbonyl)amino]methyl}piperidin-1-yl)methyl]cyclopentanecarboxylate (2.8 g, 8.0 mmol, Step 6) in MeOH (11 mL), 2 N aqueous NaOH solution (6 mL) was added at room temperature (exothermic). The resulting solution was stirred at 70° C. for 4 h, then cooled to 5˜10° C. in ice-cold water bath. To the solution, 5 N HCl aq (6 mL) was added dropwise. The resulting solution (pH value was ca.6) was concentrated and to the residue, 2-propanol (40 mL) was added. This solution was concentrated and to the residue, CH3CN (40 mL) was added. The resulting mixture was stirred at room temperature for 2 h and it was filtered through a Celite pad (5.0 g) to remove NaCl. The filtrate was concentrated to give 2.4 g (quant) of the titled compound as white solid.

1. temperaturecooled to 5˜10° C. in ice-cold water bath
2. concentrationThe resulting solution (pH value was ca.6) was concentrated and to the residue, 2-propanol (40 mL)
3. additionwas added
4. concentrationThis solution was concentrated and to the residue, CH3CN (40 mL)
5. additionwas added
6. stirringThe resulting mixture was stirred at room temperature for 2 h
7. filtrationit was filtered through a Celite pad (5.0 g)
8. customto remove NaCl
9. concentrationThe filtrate was concentrated