HRID2192919

反应详情

EQUATION

反应方程式

HRID 2192919 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 5-(2-oxoethyl)pyrazine-2-carboxylate (5.08 g) in methanol (50 mL) was added sodium borohydride (1.07 g) under ice-cooling, followed by stirring at the same temperature for 60 minutes. To the reaction mixture was added 1 M hydrochloric acid under ice-cooling to adjust the pH to 3. Saturated brine was added thereto, followed by extraction with a solvent (ethyl acetate:isopropyl alcohol=4:1). The organic layer was dried over anhydrous magnesium sulfate and concentrated. The obtained crude product was purified by silica gel column chromatography (hexane:ethyl acetate=4:1-0:1, chloroform:methanol=1:0-30:1) to obtain methyl 5-(2-hydroxyethyl)pyrazine-2-carboxylate (1.34 g) as a red-brown oily substance.

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. extractionfollowed by extraction with a solvent (ethyl acetate:isopropyl alcohol=4:1)
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe obtained crude product
  7. customwas purified by silica gel column chromatography (hexane:ethyl acetate=4:1-0:1, chloroform:methanol=1:0-30:1)