反应详情

tert-Butyl (3S)-3-[(4-{[(3,4-dichlorophenyl)amino]carbonyl}piperazin-1-yl)methyl]piperidine-1-carboxylate (1 g), trifluoroacetic acid (10 ml) and dichloromethane (20 ml) were stirred at room temperature for one hour. The solvent was removed in vacuo to yield a dark brown oil. Water (20 ml) was added to this giving a milky solution and this was then basified to ˜pH 6 by addition of solid NaHCO3. This left a milky solution which was diluted with water (˜50 ml) before extracting with ethyl acetate (3×75 ml). The combined organics were washed with brine (˜100 ml) and separated then dried (MgSO4) before removing solvent in vacuo to yield the title compound (531 mg).

1. customThe solvent was removed in vacuo
2. customto yield a dark brown oil
3. waitThis left a milky solution which
4. extractionbefore extracting with ethyl acetate (3×75 ml)
5. washThe combined organics were washed with brine (˜100 ml)
6. customseparated
7. dry with materialthen dried (MgSO4)
8. custombefore removing solvent in vacuo