HRID915613
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customa flow of anhydrous hydrochloride gas was bubbled through for 5 min
- temperatureThe solution was heated
- temperatureunder reflux for 4 hr
- customthe solvents were evaporated at low pressure
- dissolutionThe residue was dissolved in dichloromethane
- customThe reaction crude
- customwas purified by chromatography on silica gel