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
2-Chloro-6-methoxyquinoxaline (0.93 g, 4.77 mmol) and (2,4-dimethoxyphenyl)methanamine (2.2 ml, 14.64 mmol) were microwaved in dimethylsulfoxide (5 mL) for 30 min at 150° C. The reaction was diluted into ethyl acetate (250 mL) and extracted with brine (3×100 mL). The crude product was purified by column chromatography (20 to 80% ethyl acetate/hexanes) to afford N-(2,4-dimethoxybenzyl)-6-methoxyquinoxalin-2-amine (1.46 g, 87% yield). 1H NMR (400 MHz, CDCl3) δ ppm 8.13 (1H, s), 7.59-7.63 (1H, m), 7.30 (1H, d, J=8.31 Hz), 7.21-7.24 (2H, m), 6.47 (1H, d, J=2.27 Hz), 6.42 (1H, dd, J=8.31, 2.27 Hz), 5.10 (1H, t, J=5.92 Hz), 4.61 (2H, d, J=5.79 Hz), 3.88 (3H, s), 3.84 (3H, s), 3.78 (3H, s). MS (LC/MS) R.T.=1.95; [M+H]+=326.23.
WORKUP
后处理
- extractionextracted with brine (3×100 mL)
- customThe crude product was purified by column chromatography (20 to 80% ethyl acetate/hexanes)