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分别以4种离子液体为新型助溶剂,以对甲苯磺酸(Ts OH)和氯磺酸(Cl SO3H)为反应原料,以二氯乙烷为溶剂,制备了对甲苯磺酰氯(Ts Cl)。着重研究了离子液体对Ts OH在二氯乙烷和硫酸中的溶解度比s及Ts Cl产率的影响。研究结果表明,离子液体的加入可显著提高Ts OH的s值,进而提高Ts Cl的产率。在4种离子液体中,[Bu Py]BF4的效果最佳。当[Bu Py]BF4的用量为2(wt)%时,s值和Ts Cl的产率分别达12.5和87.36%。同时,考察了反应物配比、反应温度及反应时间对Ts Cl产率的影响。通过正交实验得到较优的反应条件为:n(Cl SO3H)∶n(Ts OH)为1.5∶1,反应温度为25℃,反应时间为2h。
Toluenesulfonyl chloride (TsCl) was prepared by using four kinds of ionic liquids as new cosolvents, using p-toluenesulfonic acid (Ts OH) and chlorosulfonic acid (Cl SO3H) as the starting materials and dichloroethane as solvent. . The effects of ionic liquids on the solubility of Ts OH in dichloroethane and sulfuric acid and the yield of Ts Cl were studied emphatically. The results show that the addition of ionic liquid can significantly increase the s-value of Ts OH, thereby increasing the yield of Ts Cl. Of the four ionic liquids, [Bu Py] BF4 works best. When [Bu Py] BF4 was used in an amount of 2 (wt)%, the values of s and Ts Cl were 12.5 and 87.36%, respectively. At the same time, the effects of the ratio of reactants, reaction temperature and reaction time on the yield of TsCl were investigated. The optimal reaction conditions obtained by orthogonal experiments were as follows: the molar ratio of n (Cl SO3H): n (TsOH) was 1.5:1, the reaction temperature was 25 ℃ and the reaction time was 2h.