反应详情

温度

125 °C

A mixture of the product from step 1 above (1.35 g, 5.98 mmol), piperazine (1.55 g, 17.9 mmol) and K2CO3 (0.91 g, 6.58 mmol) in acetonitrile (5 mL) was heated at 125 125° C. for 6.5 h in a sealed pyrex flask. The reaction mixture was diluted with dichlorometane, filtered and concentrated in vacuo. The semi-solid residue was purified by silica gel (16×4 cm) chromatography using CHCl3/MeOH (9:1) as eluent. Solvents were evaporated and the oily residue was redissolved in CHCl3/ether (1:1). Filtration and concentration in vacuo furnished 0.78 g (47%) of the title compound as a beige oil.

1. filtrationfiltered
2. concentrationconcentrated in vacuo
3. customThe semi-solid residue was purified by silica gel (16×4 cm) chromatography
4. customSolvents were evaporated
5. dissolutionthe oily residue was redissolved in CHCl3/ether (1:1)
6. filtrationFiltration and concentration in vacuo