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Synthesis method of 4,4'-bi-1,3-dioxolane-2,2'-dione

机译:4,4'-Bi-1,3-二氧戊烷-2,2'-二酮的合成方法

摘要

The synthesis method of 4,4'-bi-1,3-dioxolane-2,2'-dione (4,4'-BI-1,3-DIOXOLANE-2,2'-DIONE) It is a technical field in which imidazole and tetrahydrofuran are put into the reactor in an argon gas atmosphere and cooled to -5~5℃, and then phosgene starts dropping. After dropping is completed in 0.5-1h, the dropping is completed at a temperature of -8~-15℃. The mixture was dropped into a solution of tetrahydrofuran containing erythritol, and the drop was completed at 1-1.5 h. The mixture was kept warm for 0.5-2 h, and the solvent was removed by vacuum to obtain a residue. The residue was dissolved in methylene chloride, washed with cold water, dried, and concentrated to 4,4'-bi-1,3-dioxolane-2,2'-dione (4,4'-BI-1,3-DIOXOLANE). -2,2'-DIONE) 4,4'-bi-1,3-dioxolane-2,2'-DIONE (4,4'-BI-1) obtained by obtaining a crude product and refining the crude product ,3-DIOXOLANE-2,2'-DIONE) is obtained. The raw material used in the present invention is inexpensive and easily obtained, and the synthesis method is simple, so it is easy to operate, low energy consumption, short reaction time, soft and stable reaction conditions, and high product yield, and can reach 94% or more.
机译:4,4'-Bi-1,3-二氧烷氧烷-2,2'-二酮(4,4'-Bi-1,3-二氧戊烷-2,2'-Dione)的合成方法是技术领域将哪种咪唑和四氢呋喃在氩气气氛中放入反应器中并冷却至-5〜5℃,然后光源开始滴。在0.5-1H完成后掉落后,将在-8〜-15℃的温度下完成滴。将混合物滴入含有赤藓糖醇的四氢呋喃的溶液中,并在1-1.5小时内完成下降。将混合物温热0.5-2小时,并通过真空除去溶剂,得到残余物。将残余物溶于二氯甲烷中,用冷水洗涤,干燥,并浓缩至4,4'-Bi-1,3-二氧戊烷-2,2'-二酮(4,4'-Bi-1,3-二氧戊烷)。 -2,2'-dione)4,4'-Bi-1,3-二氧戊烷-2,2'-二酮(4,4'-Bi-1)通过获得粗产物获得并精炼粗产物,3获得 - 二氧氧烷-2,2'-二酮)。本发明中使用的原料是便宜的且容易获得的,合成方法简单,因此易于操作,低能耗,短反应时间,柔软且稳定的反应条件,以及高产品产量,并可到达94%以上。

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