HRID1930736

反应详情

EQUATION

反应方程式

HRID 1930736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture containing 4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (0.2 g, 0.56 mmol) and trimethylsilyl-isocyanate (0.11 ml, 0.84 mmol) in 3 ml of tetrahydrofuran is stirred for 24 hours at ambient temperature. Aminomethylpolystyrene resin EHL (Novabiochem, 200-400 mesh, 2% DVB) (200 mg, approximately 1 mmol) is added and stirring is maintained for three hours. After filtration on frit, the filtrate is concentrated in a rotavapor. Isopropyl acetate and traces of isopropanol are added to the residue obtained. The mixture is heated to dissolution followed by filtration on frit then left to crystallize for 24 hours. After filtration then drying under a bell jar, a light beige-coloured powder is obtained.

WORKUP

后处理

  1. additionAminomethylpolystyrene resin EHL (Novabiochem, 200-400 mesh, 2% DVB) (200 mg, approximately 1 mmol) is added
  2. stirringstirring
  3. temperatureis maintained for three hours
  4. filtrationAfter filtration on frit
  5. concentrationthe filtrate is concentrated in a rotavapor
  6. additionIsopropyl acetate and traces of isopropanol are added to the residue
  7. customobtained
  8. temperatureThe mixture is heated to dissolution
  9. filtrationfollowed by filtration on frit
  10. waitthen left
  11. customto crystallize for 24 hours
  12. filtrationAfter filtration
  13. customthen drying under a bell jar
  14. customa light beige-coloured powder is obtained