123664-34-6Relevant articles and documents
Method for preparing high-yield and high-purity Iguratimod intermediate
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Paragraph 0037; 0038; 0040; 0042; 0050; 0054, (2018/10/11)
The invention discloses a method for preparing an Iguratimod intermediate, i.e., 3-bromo-7-methsulfonamido-6-phenoxy-4H-1-benzo-2,3-dihydropyran-4-one. The method comprises the following steps: (1) dissolving cupric bromide in ethyl acetate and C1-C4 lower alkanol, and carrying out stirring for at least 30 minutes; (2) adding a dichloromethane solution of 7-sulfonamido-6-phenoxy-4H-1-benzo-2,3-dihydropyran-4-one into the solution obtained in the step (1), heating the temperature of the mixture to 20 DEG C to 50 DEG C with stirring, and performing a reaction for 2 to 6 hours; (3) carrying out filtering, washing filter liquor with an aqueous solution of sodium thiosulfate, and concentrating an organic phase, so as to obtain a crude product of the intermediate; and (4) carrying out refining with dichloromethane and petroleum ether, thereby obtaining a refined intermediate. The method is convenient in operation, high in conversion ratio and high in product purity, and the purity can reach96% or more.