HRID230802

反应详情

EQUATION

反应方程式

HRID 230802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An ethanol suspension (400 mL) of methyl 3-bromo-2-oxobutyrate (46.6 g) and 2-amino-5-nitropyridine (33.3 g) was stirred at 90° C. for 24 hours. The precipitated solid was taken out through filtration, and the obtained solid was suspended in ethyl acetate, washed with aqueous saturated sodium hydrogencarbonate solution, and purified through silica gel column chromatography (hexane/ethyl acetate=2/1) to obtain methyl 3-methyl-6-nitroimidazo[1,2-a]pyridine-2-carboxylate (13.0 g) as a yellow crystal.

WORKUP

后处理

  1. filtrationThe precipitated solid was taken out through filtration
  2. washwashed with aqueous saturated sodium hydrogencarbonate solution
  3. custompurified through silica gel column chromatography (hexane/ethyl acetate=2/1)