反应详情

A solution of 1-t-Butoxycarbonyl-3-(dimethylamino)methylene-4-piperidone (7.64 g, 30.04 mmol) in methanol (190 mL) was treated with guanidine carbonate (21.65 g, 120.16 mmol), followed by sodium acetate trihydrate (32.70 g, 240.32 mmol). The reaction mixture was heated at reflux for 17 hours and the solvent was removed in vacuo. The residue was diluted with water and the mixture was swirled for a few minutes. The undissolved white solid was collected and washed with water, followed by a small amount of cold ethyl acetate to give the title compound (4.10 g, 55%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 17 hours
3. customthe solvent was removed in vacuo
4. additionThe residue was diluted with water
5. waitthe mixture was swirled for a few minutes
6. customThe undissolved white solid was collected
7. washwashed with water