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
- 120 °C
PROCEDURE
实验过程
To a solution of the 4-chloro-2-isobutylimidazo[1,2-a]quinoxaline (130 mg, 0.50 mmol) in 2 mL of 1-methylpyrrolidin-2-one was added N,N-diisopropylethylamine (129 mg, 1.0 mmol) and followed by bis(4-methoxybenzyl)amine (154 mg, 0.60 mmol). The reaction mixture was stirred at 120° C. overnight. And then 10 mL of water was added. The resulting mixture was extracted with ethyl ether (50 mL×3). The combined organic layers were washed with water (20 mL), brine (20 mL), dried over MgSO4, filtered and concentrated. The crude product was purified by flash column chromatography eluted with ethyl acetate and hexanes to give the titled compound (195 mg, 81%). MS: MH+=481 1H NMR (300 MHz, CDCl3): δ 7.72 (s, 1H), 7.65 (m, 2H), 7.21-7.39 (m, 6H), 6.84 (d, 4H), 5.34 (brs, 4H), 3.79 (s, 6H), 2.63 (d, 2H), 2.06 (m, 1H), 0.94 (d, 6H).
WORKUP
后处理
- extractionThe resulting mixture was extracted with ethyl ether (50 mL×3)
- washThe combined organic layers were washed with water (20 mL), brine (20 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by flash column chromatography
- washeluted with ethyl acetate and hexanes