反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 1-(4-tert-Butoxycarbonyl-piperazin-1-yl)-4-oxo-1,9a-dihydro-4H-quinolizine-3-carboxylic acid ethyl ester (0.320 g, 0.797 mmol) in concentrated HCl (5 mL) was refluxed for 30 minutes. After cooling, the reaction was basified with aqueous NaHCO3 solution and thoroughly extracted with DCM. The combined organic layers were washed with brine, dried and concentrated to give 1-Piperazin-1-yl-1,9a-dihydro-quinolizin-4-one (0.075 g, 41%) as a yellow oil. 1H NMR (CDCl3, 400 MHz) δ 9.16 (d, J=7.2 Hz, 1H), 8.20 (d, J=9.2 Hz, 1H), 7.71 (d, J=9.6 Hz, 1H), 7.37 (t, J=7.2 Hz, 1H), 7.03 (t, J=6.4 Hz, 1H), 6.61 (d, J=9.2 Hz, 1H), 3.07 (m, 4H), 2.87 (m, 4H). LCMS (APCI+) m/z 230 [M+H]+; Rt=0.29 min.
WORKUP
后处理
- temperaturewas refluxed for 30 minutes
- temperatureAfter cooling
- extractionthoroughly extracted with DCM
- washThe combined organic layers were washed with brine
- customdried
- concentrationconcentrated