反应详情

温度

200 °C

3-Bromo-1-(4-chlorophenyl)piperazine-2,2-dimethylpropan-1-one (0.87 g, 2.43 mmol) was dissolved in N-methylpyrrolidinone (3 mL). N-Methylpiperazine (0.54 mL, 4.85 mmol) was added and the reaction mixture was heated at 200° C. for 15 minutes in a Biotage Initiator microwave at normal absorption. The reaction mixture was purified by reverse phase column chromatography (gradient eluting with MeOH in water, with 1% formic acid in each solvent, 0-30%). The resulting residue was dissolved in DCM (100 mL) and stirred with solid K2CO3 for 20 minutes, filtered and concentrated ill vacuo, to give a pale brown oil which was recrystallised from heptane to give 1-{2,2-dimethyl-3-[4-(4-chlorophenyl)piperazin-1-yl]-3-oxopropyl}-4-methylpiperazine (335 mg, 36.4%) as a white solid.

1. customThe reaction mixture was purified by reverse phase column chromatography (gradient
2. washeluting with MeOH in water, with 1% formic acid in each solvent, 0-30%)
3. dissolutionThe resulting residue was dissolved in DCM (100 mL)
4. filtrationfiltered
5. concentrationconcentrated ill vacuo
6. customto give a pale brown oil which
7. customwas recrystallised from heptane