HRID1828824

反应详情

EQUATION

反应方程式

HRID 1828824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4,5-Dibromo-2-ethylimidazole (451.3 g) was dissolved in N,N-dimethylformamide (2.25 L), and potassium carbonate (368 g) was added. (Chloromethyl)methyl ether (200 g) was gradually added dropwise under ice-cooling and the mixture was stirred at room temperature for 2 hr. The reaction mixture was poured into ice-cooled brine and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Hexane was added to the residue and the mixture was heated and allowed to cool. The precipitated crystals were collected by filtration and dried by heating under reduced pressure to give 4,5-dibromo-2-ethyl-1-(methoxymethyl)imidazole (461.7 g) as brown crystals.

WORKUP

后处理

  1. temperaturecooling
  2. additionThe reaction mixture was poured into ice-
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed successively with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. additionHexane was added to the residue
  8. temperaturethe mixture was heated
  9. temperatureto cool
  10. filtrationThe precipitated crystals were collected by filtration
  11. customdried
  12. temperatureby heating under reduced pressure