反应详情

Preparation according to Example 11: Enantiomer E1 of 3-(3,5-difluorophenyl)-pyrrolidin-3-ol (0.18 g, 0.92 mmol), formic acid (2.6 mL), aqueous formaldehyde (40%, 2.45 mL). Purification on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1) and by flash chromatography on silica gel (ethyl acetate/methanol, 10:1). Yield: 0.125 g. [α]D=+19.8° (methanol). The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether: M.p. 150° C.; MS m/z (relative intensity, 70 eV) 213 (M+, 14), 57 (bp), 58 (31), 113 (13), 127 (11), 141 (10).

1. customPreparation
2. customPurification
3. washon a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1)
4. customrecrystallized from ethanol/diethyl ether/diisopropyl ether