反应详情

To (2R)-1-(tert-butoxycarbonyl)piperazine-2-carboxylic acid (1.406 g) and Na2CO3 (2.59 g) was added dry EtOH (28 ml) then ethyl iodide (0.54 ml) and the mixture heated at reflux for 18 h under argon. The solvent was then removed under reduced pressure and 5% MeOH/DCM (40 ml) was added and stirred for 1 hour in a sealed flask. The solution was filtered and washed with dichloromethane (2×10 mL). The filtrate was then placed directly onto a 120 g-silica cartridge and was purified using eluent 10-70% MeOH/DCM. After evaporation, the product was isolated as a white foam (1.00 g), which was used without further purification.

1. temperatureat reflux for 18 h under argon
2. customThe solvent was then removed under reduced pressure and 5% MeOH/DCM (40 ml)
3. additionwas added
4. filtrationThe solution was filtered
5. washwashed with dichloromethane (2×10 mL)
6. customwas purified
7. customAfter evaporation