反应详情

温度

90 °C

A mixture of the product from step 1 above (0.93 g, 3.53 mmol) piperazine (0.88 g, 10.2 mmol) and K2CO3 (0.49 g, 3.53 mmol) in acetonitrile (7 mL) was heated in a sealed pyrex flask at 90° C. for 6.5 h. The reaction mixture was diluted with dichloromethane, filtered and concentrated in vacuo. The semi-solid residue was purified by silica gel chromatography (13×4 cm) using CHCl3/MeOH (9:1) as eluent. Solvents were evaporated off and the remaining oil was redissolved in CHCl3, filtered through a short plug of alumina, covered with K2CO3, using CHCl3 as eluent. Solvent removal in vacuo gave 0.74 g (67%) of the title compound as a beige oil. HRMS m/z calcd for C17H22N4O2 (M)+ 314.1743, found 314.1733. Anal. (C17H22N4O2.0.5H2O) C, H, N.

1. filtrationfiltered
2. concentrationconcentrated in vacuo
3. customThe semi-solid residue was purified by silica gel chromatography (13×4 cm)
4. customSolvents were evaporated off
5. dissolutionthe remaining oil was redissolved in CHCl3
6. filtrationfiltered through a short plug of alumina
7. customSolvent removal in vacuo