HRID1067663

反应详情

EQUATION

反应方程式

HRID 1067663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

5 mmol of sodium 3-(1-triphenylmethyl-1H-imidazol-4-yl)propanolate, 5 mmol of 3-methylbutane bromide and 0.5 mmol of 15-crown-15 (1, 4, 7, 10, 13-pentaoxacyclopentadecane) dissolved in 10 ml of anhydrous toluene are refluxed for 24 hours. The solvent is then evaporated off, and the residue dissolved in 10 ml THF and 30 ml 2N HCl and then heated at 70° C. for 2 hours. The THF is evaporated off under reduced pressure and triphenylmethanol is extracted with diethyl ether. The aqueous phase is neutralized with potassium carbonate and the product is extracted with diethyl ether. The organic extract is dried and evaporated, giving rise to an oil, which is crystallized as hydrogen maleate from diethyl ether and ethanol.

WORKUP

后处理

  1. temperatureare refluxed for 24 hours
  2. customThe solvent is then evaporated off
  3. dissolutionthe residue dissolved in 10 ml THF
  4. customThe THF is evaporated off under reduced pressure and triphenylmethanol
  5. extractionis extracted with diethyl ether
  6. extractionthe product is extracted with diethyl ether
  7. extractionThe organic extract
  8. customis dried
  9. customevaporated
  10. customgiving rise to an oil, which
  11. customis crystallized as hydrogen maleate from diethyl ether and ethanol