反应详情

温度

85 °C

In a 25 mL flask, tert-butyl (2R)-2-{[(2-bromophenyl)amino]carbonyl}pyrrolidine-1-carboxylate (194 mg, 0.53 mmol; which may be prepared as described in Step 1) was dissolved in DME (4 mL) under nitrogen at room temperature. CuI (6 mg, 0.03 mmol), Cs2CO3(261 mg, 0.80 mmol) and 1,10-phenanthroline (26 mg, 0.14 mmol) were added then the reaction mixture was heated at 85° C. for 24 h. The mixture was cooled to room temperature and concentrated to dryness. The residue was dissolved in dichloromethane and filtered on Celite to eliminate the cupper residue. The filtrate was concentrated and the residue purified on preparative TLC (Pentane/EtOAc, 85/15 to 50/50) to give the title compound (88 mg, 58%) as a solid.

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated to dryness
3. dissolutionThe residue was dissolved in dichloromethane
4. filtrationfiltered on Celite
5. concentrationThe filtrate was concentrated
6. customthe residue purified on preparative TLC (Pentane/EtOAc, 85/15 to 50/50)