反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAminomethylpolystyrene resin EHL (Novabiochem, 200-400 mesh, 2% DVB) (200 mg, approximately 1 mmol) is added
- stirringstirring
- temperatureis maintained for three hours
- filtrationAfter filtration on frit
- concentrationthe filtrate is concentrated in a rotavapor
- additionIsopropyl acetate and traces of isopropanol are added to the residue
- customobtained
- temperatureThe mixture is heated to dissolution
- filtrationfollowed by filtration on frit
- waitthen left
- customto crystallize for 24 hours
- filtrationAfter filtration
- customthen drying under a bell jar
- customa light beige-coloured powder is obtained