反应详情

Preparation according to Example 34: (+)-1-benzyl-3-(2,3-difluorophenyl)pyrrolidin-3-ol (0.40 g, 1.38 mmol), dimethyl formamide (3 mL), iodoethane (1.1 mL, 13.8 mmol) and morpholine (2 mL). Purification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 20:80 to 45:55). Yield: 0.11 g. [α]D=+19.8° (methanol). The amine was converted to the fumaric acid salt and recrystallized from methanol/diethyl ether/diisopropyl ether: M.p. 118-120° C.; MS m/z (relative intensity, 70 eV) 228 (M+, 14), 141, (16), 127 (14), 72 (26), 71 (bp).

1. customPreparation
2. customPurification by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 20:80 to 45:55)
3. customrecrystallized from methanol/diethyl ether/diisopropyl ether