HRID915613

反应详情

EQUATION

反应方程式

HRID 915613 的结构方程式

PROCEDURE

实验过程

A solution of 5-(2,4-difluorophenyl)-3-iodo-salicylic acid (1.69 g, 4.61 mmol) in ethanol (20 ml) was cooled to 0° C. and a flow of anhydrous hydrochloride gas was bubbled through for 5 min. The solution was heated under reflux for 4 hr and cooled to room temperature, the solvents were evaporated at low pressure. The residue was dissolved in dichloromethane and the product was worked up. The reaction crude was purified by chromatography on silica gel using hexane/ethyl acetate (7:3) as the eluent.

WORKUP

后处理

  1. customa flow of anhydrous hydrochloride gas was bubbled through for 5 min
  2. temperatureThe solution was heated
  3. temperatureunder reflux for 4 hr
  4. customthe solvents were evaporated at low pressure
  5. dissolutionThe residue was dissolved in dichloromethane
  6. customThe reaction crude
  7. customwas purified by chromatography on silica gel