HRID47441
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
2-Bromo-5-nitrobenzoic acid methyl ester (1.0 g), lithium chloride (0.49 g), tetraethyltin (0.96 g) and bis(triphenylphosphine)-palladium(II)chloride (0.1 g) were combined in dimethylformamide (20 ml) and heated at 100° C. for 8 h. Solvent was removed at reduced pressure and the residue column chromatographed (silica gel, dichloromethane/petroleum ether 30:70) to give the title compound (0.45 g). 1H NMR (CDCl3) δ: 1.28 (3H, t, J=7.4 Hz), 3.10 (2H, q, J=7.4Hz), 3.96 (3H, s), 7.47 (1H, d, J=8.5 Hz), 8.27 (1H, dd, J=2.5, 8.5 Hz), 8.73 (1H, d, J=2.5 Hz)
WORKUP
后处理
- customSolvent was removed at reduced pressure
- customthe residue column chromatographed (silica gel, dichloromethane/petroleum ether 30:70)