反应详情

温度

0 °C

Ethyl chloroformate (4.6 ml, 48.3 mmol) was added slowly to a solution of 1-(tert-butoxycarbonyl)4-piperidinecarboxylic acid (10 g, 43.6 mmol) in dichloromethane (100 ml) stirred at 0° C. Triethylamine (7.6 ml, 52.3 mmol) was added with stirring over two minutes. 0.88 Ammonia solution (40 ml) was added and the mixture allowed to warm to room temperature with stirring. The mixture was washed with water, 1M citric acid solution and brine, dried (MgSO4), filtered and evaporated under reduced pressure gave the title compound as white solid, 8.94 g.

1. stirringwith stirring over two minutes
2. temperatureto warm to room temperature
3. stirringwith stirring
4. washThe mixture was washed with water, 1M citric acid solution and brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated under reduced pressure