反应详情

To a solution of 1-(4-nitrophenyl)-piperazine (prepared as described in Reference Example 29; 13 g, 63 mmol) in acetonitrile (150 mL) were added, successively, 3-chloro-2-methyl-propene (6.82 g, 75.4 mmol) and triethylamine (17.6 mL, 126 mmol). The mixture was heated at reflux for 8 hours then the solvent was evaporated under reduced pressure to give a residue which was partitioned between water (150 mL) and ethyl acetate (2×100 mL). The combined organic layers were washed twice with water then dried over sodium sulfate. Filtration and concentration afforded 1-(2-methyl-allyl)-4-(4-nitrophenyl)-piperazine (13.2 g, 79%) as a yellow solid.

1. temperatureThe mixture was heated
2. temperatureat reflux for 8 hours
3. customthe solvent was evaporated under reduced pressure
4. customto give a residue which
5. customwas partitioned between water (150 mL) and ethyl acetate (2×100 mL)
6. washThe combined organic layers were washed twice with water
7. dry with materialthen dried over sodium sulfate
8. filtrationFiltration and concentration