反应详情

Preparation according to Example 43: Enantiomer E2 of 3-(2,3-difluorophenyl)-pyrrolidin-3-ol (0.58 g, 2.9 mmol), acetonitrile (20 mL), potassium carbonate (0.69 g, 5 mmol), cyclopropylmethyl bromide (0.308 mL, 3.18 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: 0.28 g. [α]D=−14.3° (methanol). The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether: M.p. 172.8° C.; MS m/z (relative intensity, 70 eV) 253 (M+, 4) 55 (50), 141 (18), 127 (14), 96 (bp).

1. customPreparation
2. custom2×5 min
3. customat 40° C.
4. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 4:1) Yield: 0.28 g
5. customrecrystallized from ethanol/diethyl ether