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 5 (200 mg, 0.88 mmol) and ethyl 6-iodonaphthalene-2-carboxylate (69) (194 mg, 0.62 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, 99.5/0.5, v/v) to give compound 70 (188 mg, 0.37 mmol) as a brown oil. Yield 60%; Rf (Al2O3, CH2Cl2/EtOH, 99.5/0.5, v/v) 0.47; IR (CCl4) ν 1121, 1188, 1246, 1283, 1465, 1515, 1662, 2700-3000, 3250-3400 cm−1; 1H NMR (200 MHz, CDCl3) δ 1.10 (t, 3H, J=7.1 Hz), 2.73 (q, 2H, J=7.1 Hz), 2.84 (t, 2H, J=5.7 Hz), 2.99 (t, 2H, J=5.2 Hz), 3.60 (q, 2H, J=5.7 Hz), 4.11 (t, 2H, J=5.2 Hz), 7.00 (ddd, 1H, 5JH-F=0.7 Hz, J=4.9, 7.9 Hz), 7.14 (m, 1H), 7.19 (ddd, 1H, 4JH-F=10.0 Hz, J=1.7, 7.9 Hz), 7.55 (d, 1H, J=8.6 Hz), 7.65 (m, 1H), 7.66 (d, 1H, J=8.9 Hz), 7.73 (dd, 1H, J=1.9, 8.9 Hz), 7.94 (dd, 1H, J=1.9, 8.9 Hz), 8.23 (se, 2H); ESI-MS m/z 507.9 [M+H]+.
WORKUP
后处理
- customThis compound was prepared
- customReaction time
- temperatureunder reflux
- custom12 h
- customthe purification