METHOD FOR PREPARING IMIDE DISULFURYL COMPOUND

PROBLEM TO BE SOLVED: To provide a large-scale method for preparing imide disulfuryl being a method for synthesizing a compound in the raw material of lithium bis(fluorosulfonyl)imide using no phosphorous chemical reaction, having short reaction time and a high yield, high in the purity of products...

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Hauptverfasser: CHRISTIAN SCHNIDER, STEFAN TILLE, ANDREAS KLEIN, MICHAEL GOTTSPONER, MICHAEL BITTEL, THOMAS GRUETZNER, ANNARISTINA HORMES, DOMINIQUE ROBERGE, JANINE LEIGGENER
Format: Patent
Sprache:eng ; jpn
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Zusammenfassung:PROBLEM TO BE SOLVED: To provide a large-scale method for preparing imide disulfuryl being a method for synthesizing a compound in the raw material of lithium bis(fluorosulfonyl)imide using no phosphorous chemical reaction, having short reaction time and a high yield, high in the purity of products and capable of the safe treatment of substance and reaction.SOLUTION: Provided is a method for preparing imide disulfuryl where halosulfonyl isocyanate is reacted with halosulfonic acid for 2 to 30 min at a temperature of 180 to 300°C exceeding the decomposition starting temperature of imide disulfuryl halide represented by formula (I) as a reaction product under the pressure of 50 to 500 Bar, thereafter, the reaction mixture is cooled to 0 to 150°C, and COis separated from the obtained reaction mixture. In the above method, the desired imide disulfuryl halide does not cause decomposition, the yield thereof is high, further, reaction time is short, and products show high purity.SELECTED DRAWING: None 【課題】リチウムビス(フルオロスルホニル)イミドの原料に化合物の合成方法であって、リン化学反応を使用せず、短い反応時間及び高収率を有し、生成物が高純度で、物質及び反応の安全な取扱いを可能な、大規模なイミドジスルフリルハライドの調製方法の提供。【解決手段】反応生成物である式(I)で表されるイミドジスルフリルハライドの分解開始温度を超える180〜300℃の温度と50〜500Barの圧力下で、2〜30分間、ハロスルホニルイソシアネートをハロスルホン酸と反応させ、その後、反応混合物を0〜150℃迄冷却し、得られた反応混合物からCO2を分離するイミドジスルフリルハライドの調整方法。前記方法では、所望のイミドジスルフリルハライドは分解を伴わず、それらの収率は高く、また、反応時間が短く、生成物が高純度を示すイミドジスルフリルハライドの調整方法。【選択図】なし