反应详情

温度

85 °C

A mixture of the product from step 1 above (0.94 g, 5.2 mmol), piperazine (1.28 g, 14.9 mmol, K2CO3 (0.87 g, 6.3 mmol) in acetonitrile (5 mL) was heated in a sealed pyrex flask at 85° C. for 3 h. The mixture was diluted with dichloromethane, filtered, and concentrated in vacuo. The oily residue was purified by silica gel chromatography (18×4 cm) to furnish a yellow oil. This material was redissolved in a small volume of CHCl3/ether (9:1) and filtered through a short (4 cm) plug of alumina eluting with ether/MeOH (96:4). The filtrate was concentrated in vacuo to afford 0.77 g (64%) of the title compound as a light yellow solid. HRMS m/z calcd for C12H14N4O (M)+ 230.1168, found 230.1170. Anal. (C12H14N4O) C, H, N.

1. filtrationfiltered
2. concentrationconcentrated in vacuo
3. customThe oily residue was purified by silica gel chromatography (18×4 cm)
4. customto furnish a yellow oil
5. filtrationfiltered through a short (4 cm) plug of alumina eluting with ether/MeOH (96:4)
6. concentrationThe filtrate was concentrated in vacuo