反应详情

Preparation according to Example 34: (+)-1-benzyl-3-(3-chloro-2-fluorophenyl)-pyrrolidin-3-ol (0.93 g, 3.05 mmol) and iodomethane (1 mL, 15.9 mmol), dimethyl formamid (3 mL), morpholine (2 mL). Purification by flash chromatography on silica gel (ethyl acetate/methanol, 1:0 to 1:1). Yield: 0.289 g. [α]D=+25.9° (methanol). The amine was converted to the oxalic acid salt and recrystallized from methanol/diethyl ether/diisopropyl ether: M.p. 123-125° C.; MS m/z (relative intensity, 70 eV) 229 (M+, 7), 157 (8), 129 (6), 58 (29), 57 (bp).

1. customPreparation
2. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 1:0 to 1:1)
3. customrecrystallized from methanol/diethyl ether/diisopropyl ether