反应详情

温度

130 °C

To 4-2[-amino-1-(2-chloro-phenyl)-ethyl]-1-Boc-piperazine (201) (4.34g, 12.7 mmol) was added phthalic anhydride (1.89 g, 12.7 mmol). The mixture was heated at 130° C. for 1 h and then allowed to cool to room temperature. The resulting solid was recrystallized from MeOH. The enantiomers of the phthalimide-protected product were separated by chiral chromatography, using a Chiralcel OD (4.6×250 mm) column, eluting with 5% 3A alcohol in heptane at 1 mL/min. The first eluting isomer was labeled isomer #1 and the second eluting isomer #2. 5.6 g (95%) of the mixture was isolated and separated.

1. temperatureto cool to room temperature
2. customThe resulting solid was recrystallized from MeOH
3. customThe enantiomers of the phthalimide-protected product were separated by chiral chromatography
4. washeluting with 5% 3A alcohol in heptane at 1 mL/min