HRID1916376

反应详情

EQUATION

反应方程式

HRID 1916376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1H-imidazole-2-carboaldehyde (2.0 g), N-methylpyrrolidone (25 mL) was added, followed by dissolution with heating. To the resultant solution, ethyl chloroacetate (11.1 mL) and potassium carbonate (2.9 g) were added. The reaction solution was stirred at room temperature for 14 hours. To the reaction solution, water (30 mL) was added. The aqueous layer was extracted twice with ethyl acetate. The organic layers were combined, washed with saturated saline and then dried over anhydrous sodium sulfate. The anhydrous sodium sulfate was removed by filtration and the solvent was concentrated under reduced pressure. The residue was purified by silica gel chromatography (dichloromethane) to obtain the title compound having the following physical properties (1.3 g).

WORKUP

后处理

  1. dissolutionfollowed by dissolution
  2. temperaturewith heating
  3. extractionThe aqueous layer was extracted twice with ethyl acetate
  4. washwashed with saturated saline
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe anhydrous sodium sulfate was removed by filtration
  7. concentrationthe solvent was concentrated under reduced pressure
  8. customThe residue was purified by silica gel chromatography (dichloromethane)