HRID1930740

反应详情

EQUATION

反应方程式

HRID 1930740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

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 isopropylisocyanate (0.155 g, 1.8 mmol) in 3 ml of dimethylformamide is heated at 100° C. for two hours then stirred at ambient temperature for two hours. 20 ml of water and 30 ml of ethyl acetate are added, followed by extraction, then the organic phase is washed with a saturated sodium chloride solution. The organic phase is dried over sodium sulfate. After evaporation to dryness, the oil obtained is triturated in isopentane. After filtration then drying, the solid obtained is purified on a silica column (eluent dichloromethane-ethanol-ammonia 96/2/2) and a pink-cream coloured powder is obtained with a yield of 20%.

WORKUP

后处理

  1. extractionfollowed by extraction
  2. washthe organic phase is washed with a saturated sodium chloride solution
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customAfter evaporation to dryness
  5. customthe oil obtained
  6. customis triturated in isopentane
  7. filtrationAfter filtration
  8. customthen drying
  9. customthe solid obtained
  10. customis purified on a silica column (eluent dichloromethane-ethanol-ammonia 96/2/2)
  11. customis obtained with a yield of 20%