HRID1165137

反应详情

EQUATION

反应方程式

HRID 1165137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.35 g of 1-amino-2-methylimidazole hydrochloride are dissolved in 300 ml of ethanol, whereupon 9.3 g of 4-hydroxy-3,5-di-tert.-butylbenzaldehyde are added. The mixture is stirred at room temperature for 1 hour and then evaporated in a vacuum. 150 ml of ice-water and 200 ml of methylene chloride are added to the residue and the mixture is neutralized (pH=7) with saturated sodium bicarbonate solution. The methylene chloride phase is separated and the aqueous phase is extracted with 100 ml of methylene chloride. The combined methylene chloride phases are dried and evaporated. The residue is stirred with ether and filtered. The filter residue is dried at 80° in a vacuum and there is obtained 1-(4-hydroxy-3,5-di-tert.-butylbenzylideneamino)-2-methylimidazole of m.p. 206°-207°.

WORKUP

后处理

  1. additionare added
  2. customevaporated in a vacuum
  3. addition150 ml of ice-water and 200 ml of methylene chloride are added to the residue
  4. customThe methylene chloride phase is separated
  5. extractionthe aqueous phase is extracted with 100 ml of methylene chloride
  6. dry with materialThe combined methylene chloride phases are dried
  7. customevaporated
  8. stirringThe residue is stirred with ether
  9. filtrationfiltered
  10. customThe filter residue is dried at 80° in a vacuum