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), 1,1,1-trifluoro-3-iodopropane (0.32 mL, 3.1 mmol). Stirred 2 h at ambient temperature and 2×5 min at 40° C.; Purification by flash chromatography on silica gel (ethyl acetate/methanol, 4:1) Yield: 0.2 g. [α]D=−14.6° (methanol). The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether: M.p. 144° C.; MS m/z (relative intensity, 70 eV) 295 (M+, 24), 212 (31), 182 (12), 139 (bp), 127 (20).

1. customPreparation
2. custom2×5 min
3. customat 40° C.
4. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 4:1) Yield: 0.2 g
5. customrecrystallized from ethanol/diethyl ether