HRID1019044

反应详情

EQUATION

反应方程式

HRID 1019044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 4-[(E)-3-(1-tritylimidazol-5-yl)prop-1-en-1-yl]-2-(4-fluorophenyl)benzoate (7.8 g; 10 mmol), 12N HCl (7.5 ml) and acetic acid (7.5 ml) in methanol (150 ml) was refluxed for 1 hour 30 minutes. After evaporation to dryness and neutralisation with an aqueous solution of ammonium hydroxide, the residue was extracted with dichloromethane and purified by flash chromatography, eluting with a gradient 2-5% ethanol/dichloromethane to give methyl 4-[(E)-3-(imidazol-5-yl)prop-1-en-1-yl]-2-(4-fluorophenyl)benzoate. Yield: 20%.

WORKUP

后处理

  1. customAfter evaporation to dryness and neutralisation with an aqueous solution of ammonium hydroxide
  2. extractionthe residue was extracted with dichloromethane
  3. custompurified by flash chromatography
  4. washeluting with a gradient 2-5% ethanol/dichloromethane