反应详情

A mixture of 1-fluoro-4-nitrobenzene (2.54 mL, 24 mmol) and N-methylpiperazine (2.22 mL, 20 mmol) was dissolved in DMSO (25 mL) and irradiated in a microwave oven (max power 250 W, 160° C.) for 10 min, then cooled to room temperature. The solvent was removed under high vacuum, and the residue was dissolved in EtOAc and extracted with 0.5M aqueous HCl. The aqueous extracts were combined, basified to pH 8, and extracted with EtOAc. The organic layer was washed with brine, and then dried over MgSO4. Evaporation of the solvent provided the crude 1-methyl-4-(4-nitrophenyl)piperazine as an brown oil.

1. customirradiated in a microwave oven (max power 250 W, 160° C.) for 10 min
2. customThe solvent was removed under high vacuum
3. dissolutionthe residue was dissolved in EtOAc
4. extractionextracted with 0.5M aqueous HCl
5. extractionextracted with EtOAc
6. washThe organic layer was washed with brine
7. dry with materialdried over MgSO4
8. customEvaporation of the solvent