反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
This compound was prepared, starting from compound 59 (600 mg, 2.36 mmol), according to the procedure developed for compound 10. Reaction time under reflux: 12 h; the purification was performed using column chromatography (Al2O3, CH2C2/EtOH, 99/1, v/v) to give compound 60 (902 mg, 1.68 mmol) as a light sensitive brown oil. Yield 71%; Rf (Al2O3, CH2Cl2/EtOH, 99/1, v/v) 0.46; IR (CCl4) ν 1117, 1289, 1526, 1549, 1683, 2800-3000, 3410 cm−1; 1H NMR (200 MHz, CDCl3) δ 1.08 (t, 3H, J=7.1 Hz), 2.70 (q, 2H, J=7.1 Hz), 2.83 (t, 2H, J=6.1 Hz), 2.99 (t, 2H, J=5.3 Hz), 3.57 (q, 2H, J=6.1 Hz), 4.17 (t, 2H, J=5.3 Hz), 7.36 (dd, 1H, J=4.2, 8.4 Hz), 7.43 (dd, 1H, J=1.7, 8.4 Hz), 7.61 (d, 1H, J=8.8 Hz), 7.94 (dd, 1H, J=1.7, 4.2 Hz), 7.99 (dd, 1H, J=1.8, 8.8 Hz), 8.29 (m, 1H), 8.53 (d, 1H, J=1.8 Hz), 9.57 (s, 1H); ESI-MS m/z 536.9 [M+H]+.
WORKUP
后处理
- customThis compound was prepared
- customReaction time
- temperatureunder reflux
- custom12 h
- customthe purification