反应详情

温度

60 °C

A suspension of (trans)-4-aminocyclohexanecarboxylic acid (5 g, 34.9 mmol) in EtOH (100 mL, 1713 mmol) was treated with HCl (9.09 mL, 105 mmol) and the mixture was stirred at 60° C. overnight. The reaction mixture turned to clear solution. It was concentrated under reduced pressure and the residue was triturated with Et2O in CH3CN (50%) and the resulting white solid was collected. There was some product left in the filtrate so it was concentrated and triturated with Et2O in CH3CN (50%), the white solid was collected by filtration and combined with the white solid that was collected previously to provide 13A.HCl (5.25 g, 25.3 mmol, 72.4% yield). 1H NMR (400 MHz, CDCl3) δ ppm 4.06 (q, 2H, J=7.1 Hz); 3.01-3.15 (m, 1H); 1.34-2.31 (m, 9H); 1.18 (t, 3H, J=7.1 Hz).

1. concentrationIt was concentrated under reduced pressure
2. customthe residue was triturated with Et2O in CH3CN (50%)
3. customthe resulting white solid was collected
4. waitleft in the filtrate so it
5. concentrationwas concentrated
6. customtriturated with Et2O in CH3CN (50%)
7. filtrationthe white solid was collected by filtration
8. customthat was collected previously