反应详情

温度

140 °C

2-[2-(4-tert-Butoxycarbonyl-piperazin-1-yl)-1-ethoxy-2-pyridin-2-yl-ethyl]-malonic acid diethyl ester (2.40 g, 4.86 mmol) was dissolved in xylene (20 mL) and heated at 140° C. for 12 hours. After cooling, the volatiles were evaporated and the residue was purified by column chromatography (EtOAc) to give 1-(4-tert-Butoxycarbonyl-piperazin-1-yl)-4-oxo-1,9a-dihydro-4H-quinolizine-3-carboxylic acid ethyl ester (1.39 g, 71%) as an orange solid. 1H NMR (CDCl3, 400 MHz) δ 9.48 (d, J=7.2 Hz, 1H), 8.34 (s, 1H), 7.69 (td, J=7.2 Hz, J=1.2 Hz, 1H), 7.23 (m, 1H), 4.44 (q, J=7.2 Hz, 2H), 4.14 (m, 2H), 3.10 (m, 2H), 2.88 (m, 4H), 1.51 (s, 9H), 1.43 (t, J=7.2 Hz, 3H). LCMS (APCI+) m/z 402 [M+H]+; Rt=2.85 min.

1. temperatureAfter cooling
2. customthe volatiles were evaporated
3. customthe residue was purified by column chromatography (EtOAc)