HRID1067667

反应详情

EQUATION

反应方程式

HRID 1067667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 mmol of 3-phenylpropyltriphenylphosphonium bromide, 10 mmol of (1-triphenylmethyl-1H-imidazol-4-yl)methanal (J. L. Kelley, C. A. Miller, E. W. Mc Lean, J. Med. Chem. 1977, 20, 721) and 12 mmol of potassium of t-butanolate are stirred for 24 hours in 50 ml THF. The solvent is evaporated off under reduced pressure, hydrolysed with water and extracted using chloroform. The concentrated organic extract is heated from reflux in 30 ml 2N HCl and 30 ml of acetone for 1 hour. The solvent is evaporated off under reduced pressure and triphenylmethanol is extracted using diethyl ether. The aqueous phase is alkalized using ammonia and the crude product is extracted using diethyl ether. The aqueous phase is alkalized using diethyl ether and crystallized as hydrogen maleate from diethyl ether and ethanol.

WORKUP

后处理

  1. customThe solvent is evaporated off under reduced pressure, hydrolysed with water
  2. extractionextracted
  3. extractionThe concentrated organic extract
  4. temperatureis heated
  5. temperaturefrom reflux in 30 ml 2N HCl
  6. customThe solvent is evaporated off under reduced pressure and triphenylmethanol
  7. extractionis extracted
  8. extractionthe crude product is extracted
  9. customcrystallized as hydrogen maleate from diethyl ether and ethanol