反应详情

温度

80 °C

Into a 30 mL vial, 1-(2-Bromo-ethoxy)-4-nitro-benzene (5.00 g, 0.0203 mol), piperazine, 1-methyl-(4.51 mL, 0.0406 mol), Acetonitrile (15.0 mL, 0.287 mol) and Potassium carbonate (5.62 g, 0.0406 mol) were added. The reaction was heated at 80° C. for 4 hours. The reaction was partitioned with water and extracted with Et2O (3×100 mL). The Combined organic was washed with Brine, and dried over magnesium sulfate. The solid was filtered and washed with EtOAc. The solvent was removed under vacuum to afford 1-Methyl-4-[2-(4-nitro-phenoxy)-ethyl]-piperazine as an off white solid (3.89 g, 73%). NMR 1H (DSMO-d6-8.20 (dd, 2H, JJ=2.04, 5.12 Hz), 7.16 (dd, 2H, JJ=2.04, 5.08 Hz), 4.22 (t, 2H, J=5.76 Hz), 2.71 (t, 2H, J=5.72 Hz), 2.18-2.6 (bm, 8H), 2.13 (s, 3H)

1. customThe reaction was partitioned with water
2. extractionextracted with Et2O (3×100 mL)
3. washThe Combined organic was washed with Brine
4. dry with materialdried over magnesium sulfate
5. filtrationThe solid was filtered
6. washwashed with EtOAc
7. customThe solvent was removed under vacuum