HRID1403540
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
- 80 °C
PROCEDURE
实验过程
To a solution of methyl 3-chloro-2-oxo-1,2-dihydroquinoxaline-6-carboxylate (150 mg, 0.63 mmol) in DMSO (2 mL) was added (S)-2-methylpiperidine (166 mg, 1.7 mmol) and DIEA (217 mg, 1.7 mmol). The resulting solution was stirred for 3 hours at 80° C. and then quenched by the addition of water (250 mL), extracted with dichloromethane (3×100 mL), dried over anhydrous sodium sulfate, and then concentrated under vacuum to give a residue, which was purified via silica gel column chromatography (9% ethyl acetate in petroleum ether) to afford (S)-methyl 3-(2-methylpiperidin-1-yl)-2-oxo-1,2-dihydroquinoxaline-6-carboxylate as white solid (165 mg, 87%).
WORKUP
后处理
- customquenched by the addition of water (250 mL)
- extractionextracted with dichloromethane (3×100 mL)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under vacuum
- customto give a residue, which
- customwas purified via silica gel column chromatography (9% ethyl acetate in petroleum ether)