HRID1403540

反应详情

EQUATION

反应方程式

HRID 1403540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched by the addition of water (250 mL)
  2. extractionextracted with dichloromethane (3×100 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under vacuum
  5. customto give a residue, which
  6. customwas purified via silica gel column chromatography (9% ethyl acetate in petroleum ether)