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    A METHOD FOR PREPARATION OF PERFLUOROALKYL SULFENYL CHLORIDE
    9.
    发明公开
    A METHOD FOR PREPARATION OF PERFLUOROALKYL SULFENYL CHLORIDE 有权
    一种制备全氟烷基硫醚氯化物的方法

    公开(公告)号：EP2521712A1

    公开(公告)日：2012-11-14

    申请号：EP10840705.7

    申请日：2010-06-08

    申请人： Gharda, Keki Hormusji

    发明人： Gharda, Keki Hormusji

    IPC分类号： C07C313/08 ,  C07C313/02 ,  C07C313/00 ,  C07C319/14

    CPC分类号： C07C313/08 ,  B01F3/1271 ,  B01F5/10 ,  B01F7/00633 ,  B01F7/18 ,  B01F15/066 ,  B01F2015/061 ,  B01J8/20 ,  B01J19/0066 ,  B01J19/1881 ,  B01J2219/00063 ,  B01J2219/00065 ,  B01J2219/00081 ,  C07C319/14 ,  C07C323/07

    摘要： Preparing perfluoromethyl sulfenyl chloride involves reacting halogenated aromatic compound with fluoride compounds e.g. potassium bifluoride and sodium fluoride, and thiophosgene in a solvent e.g. acetonitrile; pulverizing the reaction mass by using beads e.g. glass and/or zirconium oxide beads; isolating trifluoromethyl thiomethyl benzene derivative from the mixture; distilling the benzene derivative; dissolving purified benzene derivative in a solvent e.g. dichloromethane; and cleaving the benzene derivative by selective chlorinolysis by passing chlorine gas at -10 to 30[deg] C. Preparation of perfluoromethyl sulfenyl chloride involves reacting halogenated aromatic compound of formula R'-CH 2-R (I) with at least one fluoride compound selected from potassium fluoride, potassium bifluoride, sodium fluoride, tetramethylammonium fluoride and benzyltrimethylammonium fluoride and thiophosgene in a solvent selected from acetonitrile, dichloromethane, sulfolane and carbon tetrachloride to obtain a reaction mass; pulverizing the reaction mass with the help of beads selected from glass, sand, stainless steel, titanium and/or zirconium oxide beads to obtain a mixture containing trifluoromethyl thiomethyl benzene derivative; isolating the trifluoromethyl thiomethyl benzene derivative from the mixture; distilling the trifluoromethyl thiomethyl benzene derivative to obtain a purified trifluoromethyl thiomethyl benzene derivative; dissolving the purified trifluoromethyl thiomethyl benzene derivative in a solvent selected from dichloromethane, toluene, benzene, ethylene dichloride, mono chloro benzene, carbon tetrachloride, ortho dichloro benzene and trichloro benzene; and cleaving the trifluoromethyl thiomethyl benzene derivative by selective chlorinolysis by passing chlorine gas at -10 to 30[deg] C. R : optionally substituted aromatic group; R' : halo selected from fluoro, chloro, bromo and iodo. An independent claim is included for a system for the preparation of perfluoromethyl sulfenyl chloride comprising a reactor containing an inlet for facilitating entry of reactants into the reactor, an outlet for facilitating exit of final product out of the reactor, a stirrer for mixing the reactants contained inside the reactor, a cooler for preventing overheating of the reactants, a temperature measuring and indicating unit for measuring and indicating the temperature of the resulting mixture of the reactants contained inside the reactor, and a pressure gauge for measuring pressure generated inside the reactor; a pump for moving the resulting mixture contained inside the reactor; and a bead mill comprising beads for pulverization of the resulting mixture moved from the gear pump, where the pulverized mixture enter into the reactor for further mixing; and the final product formed after subsequent mixing is existed through the outlet of the reactor.

    摘要翻译： 制备全氟甲基亚磺酰氯包括使卤代芳族化合物与氟化合物例如 二氟化钾和氟化钠，以及溶剂中的硫光气。 乙腈; 通过使用例如珠粒来粉碎反应物质。 玻璃和/或氧化锆珠; 从混合物中分离三氟甲基硫代甲基苯衍生物; 蒸馏苯衍生物; 将纯化的苯衍生物溶解在溶剂中，例如， 二氯甲烷; 并通过在-10至30℃使氯气通过选择性氯解来裂解苯衍生物。全氟甲基亚磺酰氯的制备包括使式R'-CH 2 -R（I）的卤代芳族化合物与至少一种氟化合物 在选自乙腈，二氯甲烷，环丁砜和四氯化碳的溶剂中选自氟化钾，氟化钾，氟化钠，氟化四甲基铵和苄基三甲基氟化铵和硫光气以获得反应物质; 在选自玻璃，沙子，不锈钢，钛和/或氧化锆珠的珠的帮助下粉碎反应物料以获得含有三氟甲基硫代甲基苯衍生物的混合物; 从混合物中分离三氟甲基硫代甲基苯衍生物; 蒸馏三氟甲基硫代甲基苯衍生物得到纯化的三氟甲基硫代甲基苯衍生物; 将纯化的三氟甲基硫代甲基苯衍生物溶解在选自二氯甲烷，甲苯，苯，二氯乙烷，一氯苯，四氯化碳，邻二氯苯和三氯苯的溶剂中; 并通过在-10至30℃通过氯气进行选择性氯解，裂解三氟甲基硫代甲基苯衍生物。R：任选取代的芳族基团; R'：选自氟，氯，溴和碘的卤素。 包括用于制备全氟甲基亚磺酰氯的系统的独立权利要求包括含有用于促进反应物进入反应器的入口的反应器，用于促进最终产物离开反应器的出口，用于混合包含的反应物的搅拌器 用于防止反应物过热的冷却器，用于测量和指示反应器内所含反应物的所得混合物的温度的温度测量和指示单元以及用于测量反应器内产生的压力的压力计; 用于移动反应器内所含混合物的泵; 和包含用于粉碎所得混合物的珠粒的珠磨机，所述珠粒磨粉机从所述齿轮泵运动，其中所述粉碎混合物进入所述反应器用于进一步混合; 并且随后混合后形成的最终产物通过反应器的出口存在。