反应详情

Preparation according to Example 43: Enantiomer E2 of 3-(2,3-difluorophenyl)-pyrrolidin-3-ol (0.5 g, 2.5 mmol), acetonitrile (20 mL), potassium carbonate (0.69 g, 5 mmol), 1-bromo-2-methoxyethane (0.255 mL, 2.7 mmol). Stirred 1 h at ambient temperature. Addition of 1-bromo-2-methoxyethane (0.05 mL, 0.53 mmol), stirred at 40° C. for 2 min. Purification by flash chromatography on silica gel (ethyl acetate/methanol, 4:1). Yield: 0.32 g. [α]D=−20.8° (methanol). The amine was converted to the oxalic acid salt and recrystallized from methanol/diisopropyl ether: M.p. 146.7° C.; MS m/z (relative intensity, 70 eV) 257 (M+, 2), 212 (bp), 182 (56), 141 (9), 127 (12).

1. customPreparation
2. stirringstirred at 40° C. for 2 min
3. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 4:1)
4. customrecrystallized from methanol/diisopropyl ether