反应详情

Preparation according to Example 26: 3-(3-chloro-2-fluorophenyl)-pyrrolidin-3-ol (0.6 g, 2.78 mmol), formic acid (8.1 mL), aqueous formaldehyde (40%, 7.2 mL). Purification by flash chromatography on silica gel (ethyl acetate/methanol, 2:8 to 3:8) and by HPLC on Waters OBD C18, 5 μm (MeOH/33 mM NH3, 20:80 to 100:0). Yield: 0.3 g. The amine was converted to the fumaric acid salt and evaporated to a solid residue: MS m/z (relative intensity, 70 eV) 229 (M+, 10), 157 (8), 129 (5), 58 (28), 57 (bp).

1. customPreparation
2. customPurification by flash chromatography on silica gel (ethyl acetate/methanol, 2:8 to 3:8)
3. customevaporated to a solid residue