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发明授权
CN101302213B 顺式-2-(2，4-二氯苯基)-2-([1，2，4]-三唑-1-甲基)-[1，3]二氧戊环-4-甲基甲磺酸酯的制备方法 失效 - 权利终止 许可

顺式-2-(2，4-二氯苯基)-2-([1，2，4]-三唑-1-甲基)-[1，3]二氧戊环-4-甲基甲磺酸酯的制备方法
摘要：
本发明涉及医药中间体顺式-2-(2，4-二氯苯基)-2-([1，2，4]三唑-1-甲基)-[1，3]二氧戊环-4-甲基甲磺酸酯的制备方法。采用以间二氯苯为原料的工艺路线，经付-克反应、在杂多酸TiSiW12O40/SiO2催化下与甘油缩合、苯甲酰氯酯化、在碳酸钠催化下与1，2，4-三氮唑缩合、水解重结晶、甲磺酰氯酯化得到产品。其特点是：(1)采用独创的以间二氯苯为原料的工艺路线；(2)缩酮的生产采用杂多酸TiSiW12O40/SiO2催化，可重复利用，具有环保性和经济性；(3)采用碳酸钠作缚酸剂，避免采用昂贵、危险的氢化钠催化；(4)采用重结晶方法避免了柱层析，生产成本降低且利于工业化。
摘要（英）：

The invention relates to a preparation method for pharmaceutical intermediate cis-2-(2,4- dichlorophenyl)-2-([1,2,4]triazole-1-methyl)-[1,3] dioxolane-4-methyl methanesulfonate. The preparation method adopts a process route that m-dichlorobenzene is used as a raw material which is condensed with glycerin under the catalysis of heteropoly acid TiSiW12O40/SiO2 after friedel-crafts reaction, and is esterified with benzoyl chloride, and the product is obtained by condensing the reaction product with 1,2,4-triazole, hydrolyzing, recrystallizing and esterifying with the methylsulfonyl chloride. The invention is characterized by (1) adopting a creative process route that the m-dichlorobenzene is used as the raw material; (2) adopting the heteropoly acid TiSiW12O40/SiO2 for catalysis in the production of ketal, the heteropoly acid being repeated and having environmental and economical performances; (3) adopting sodium carbonate as an acid binding agent, avoiding the expensive and dangerous sodium hydride catalysis; and (4) adopting a recrystallization method and avoiding column chromatography, lowering the production cost and being useful for industrialization.

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