| 徐聪,周大鹏,刘丹,吴建一.化学通报,2016,79(9):860-863. |
| 用离子液助溶剂制备对甲苯磺酰氯 |
| Preparation of p-Toluene Sulfonyl Chloride Using Ionic Liquid as Co-solvent |
| 投稿时间：2016-01-08 修订日期：2016-03-23 |
| DOI： |
| 中文关键词: 离子液对甲苯磺酰氯酰氯化溶解度比 |
| 英文关键词:Ionic liquids, p-Toluene sulfonyl chloride, Sulfonyl chloride reaction, Solubility ratio |
| 基金项目:嘉兴市科技计划项目(2014AY11023)和浙江省芳烃磺酸工程技术研究中心开放基金项目(84214001-1)资助 |
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| 中文摘要: |
| 分别以4种离子液为新型助溶剂，以对甲苯磺酸（TsOH）和氯磺酸（ClSO3H）为反应原料，以二氯乙烷为溶剂，制备了对甲苯磺酰氯（TsCl）。着重研究了离子液对TsOH在二氯乙烷和硫酸中的溶解度比s及TsCl产率的影响。研究结果表明，离子液的加入可显著提高TsOH的s值，进而提高TsCl的产率。在4种离子液中，[BuPy]BF4的效果最佳。当[BuPy]BF4的用量为2（wt）%时，s值和TsCl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TsCl产率的影响。通过正交实验得到较优的反应条件为：n(ClSO3H):n(TsOH)为1.5:1，反应温度为25℃，反应时间为2h。 |
| 英文摘要: |
| Four kinds of different ionic liquids were investigated as novel co-solvents for synthesis of p-toluene sulfonyl chloride (TsCl) with p-toluene sulfonyl acid (TsOH) and chlorosulfonic acid (ClSO3H) as feedstocks in ethylidene chloride. The effect of ionic liquids on solubility ratio (s value) of TsOH in ethylidene chloride and sulphuric acid, as well as the yield of TsCl was studiedparticularly. The results showed that the s value of TsOH was significantly enhanced with increasing of ionic liquid amount. The yield of TsCl thus was also increased, correspondingly. Among four screened ionic liquids, [BuPy]BF4was proved to be the best co-solvent. The s value of TsOH and the yield of TsCl at optimal [BuPy]BF4content (2(wt)%) were 12.5 and 87.36%, respectively. The influence of the molar ratio of feedstocks, reaction temperature and reaction time on the yield of TsCl were also investigated. The optimum reaction conditions that determined by orthogonal experiment were follows: n(ClSO3H): n(TsOH) =1.5:1, reaction temperature is 25℃, reaction time is 2h. |
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