反应详情

温度

0 °C

To a solution of (R,S)2-(1-pyrrolidinyl)methyl]piperazine hydrochloride (1.0 g, 3.58 mmol) and Et3N (0.5 mL, 3.58 mmol) in 10 mL of CH2Cl2 was added trifluoroacetic anhydride (0.5 mL, 3.58 mmol) at 0° C. The reaction mixture is stirred at 0° C. for 5 h. The reaction mixture was evaporated under reduced pressure (due to the water solubility of this compound there was no aqueous work-up) and isolated on a silica gel column (solvent system: CH2Cl2: CH3OH: 28% NH4OH (98:2:2) to give the desired product as a free base (0.18 g, 20%); 1H NMR (free base 200 MHz, CDCl3) d 1.76 (m,4H), 2.25-3.15 (m, 10H), 3.26 (t, 2H), 3.88 (m, 1H), 4.39 (t, 1H).

1. customThe reaction mixture was evaporated under reduced pressure (due to the water solubility of this compound there
2. customisolated on a silica gel column (solvent system