反应详情

Preparation according to Example 11: Enantiomer E2 of 3-(3,5-difluorophenyl)-pyrrolidin-3-ol (0.29 g, 1.45 mmol), formic acid (3.8 mL), aqueous formaldehyde (40%, 3.4 mL). 65° C. for 5 h. Purification by flash chromatography on silica gel (ethyl acetate/methanol, 10:1). Yield: 0.19 g. [α]D=−22.8° (methanol). The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether: M.p. 134-135° C.; MS m/z (relative intensity, 70 eV) 213 (M+, 15), 57.1 (bp), 58.1 (31), 113 (13), 127 (11), 141 (11).

1. customPreparation
2. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 10:1)
3. customrecrystallized from ethanol/diethyl ether/diisopropyl ether