反应详情

In acetonitrile (80 ml), tert-butyl 1-piperazine carboxylate (2.50 g) was dissolved. Under ice cooling, benzyl bromide (1.59 ml) and triethylamine (1.87 ml) were added dropwise to the resulting solution, followed by stirring at room temperature for 90 minutes. After the solvent was distilled off under reduced pressure, distilled water and dichloromethane were added to the residue to separate the organic layer. The organic layer was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (ethyl acetate:hexane=1:20 to 1:5), whereby the title compound (3.12 g, 84%) was obtained as colorless powder.

1. distillationAfter the solvent was distilled off under reduced pressure
2. distillationdistilled water and dichloromethane
3. additionwere added to the residue
4. customto separate the organic layer
5. washThe organic layer was washed with saturated aqueous NaCl solution
6. dry with materialdried over anhydrous sodium sulfate
7. customThe residue obtained
8. distillationby distilling off the solvent under reduced pressure
9. customwas purified by chromatography on a silica gel column (ethyl acetate:hexane=1:20 to 1:5), whereby the title compound (3.12 g, 84%)
10. customwas obtained as colorless powder