反应详情

Preparation according to Example 24: Enantiomer E1 of 3-(3,5-difluorophenyl)-pyrrolidin-3-ol (0.53 g, 2.66 mmol), acetonitrile (3 mL), potassium carbonate (0.55 g, 3.99 mmol) and iodopropane (260 μl, 2.66 mmol). Purification by HPLC on Waters OBD 018, 5 μm (MeOH/33 mM NH3, 40:60 to 60:40). Yield: 0.274 g. [α]D=+21.2° (methanol). The amine was converted to the oxalic acid salt and recrystallized from methanol/diethyl ether: M.p. 117-118° C.; MS m/z (relative intensity, 70 eV) 241 (M+, 8), 212, (bp), 182 (35), 127 (12), 84 (45).

1. customPreparation
2. customPurification by HPLC on Waters OBD 018, 5 μm (MeOH/33 mM NH3, 40:60 to 60:40)
3. customrecrystallized from methanol/diethyl ether