反应详情

温度

110 °C

A mixture of the product from Step 1 above (1.07 g, 3.90 mmol), piperazine (0.98 g, 11.3 mmol) and K2CO3 (0.54 g, 3.9 mmol) in acetonitrile (11 mL) was heated at 85° C. for 5 h and at 110° C. for 8 h in a sealed pyrex flask. The reaction mixture was diluted with CHCl3, filtered, and concentrated in vacuo. The semi-solid residue was purified by chromatography on silica gel (11×4 cm) using CHCl3/MeOH (9: 1) as eluent. The resulting oil was redissolved in CHCl3 and filtered through a short plug of alumina, covered by K2CO3, using CHCl3 as eluent. Solvent removal in vacuo furnished 0.50 g (23%) of the title compound as an oil that solidified upon standing: mp 133-135° C. HRMS m/z calcd for C18H21N5O (M)+ 323.1746, found 323.1763. Anal. (C18H21N5O) C, H, N.

1. filtrationfiltered
2. concentrationconcentrated in vacuo
3. customThe semi-solid residue was purified by chromatography on silica gel (11×4 cm)
4. dissolutionThe resulting oil was redissolved in CHCl3
5. filtrationfiltered through a short plug of alumina
6. customSolvent removal in vacuo