A SIMPLE AND FAST PROCEDURE FOR EFFICIENT SYNTHESIS OF DISIDA AND ITS DERIVATIVES OR MEBROFENIN USING MICROWAVE IRRADIATION

摘要

Provided is a method for preparing DISIDA and derivatives thereof or mebrofenin using microwave irradiation, whereby DISIDA and derivatives thereof or mebrofenin is easily obtained in high yield within very short reaction time and the load of environmental pollution is reduced. The method for preparing DISIDA and derivatives thereof using microwave irradiation comprises the steps of: (1) putting a glacial acetic acid solution containing 2,6-diisopropylaniline and chloroacetyl chloride into a microwave-irradiating container to apply microwaves to the solution, thereto adding an aqueous solution of sodium acetate trihydrate to precipitate products, performing filtration and drying, and recrystallizing the dried precipitates with ethanol to obtain 2,6-diisopropyl-chloroacetanilide and derivatives thereof; and (2) dissolving the compound and derivatives thereof and iminodiacetic acid disodium salt in an aqueous ethanol solution, thereto adding sodium hydroxide for pH control, putting the prepared solution into a microwave-irradiating container to apply microwaves to the solution, cooling the solution to room temperature, removing ethanol from the solution, extracting the water layer with diethyl ether, precipitating products while adjusting pH of the water layer to about 2-3 using conc. HCl, performing filtration and drying, and recrystallizing the dried precipitates with ethanol to obtain N-(2,6-diisopropylacetanilido)-aminodiacetic acid(DISIDA) and derivatives thereof.