机械力促进的硫醚选择性氧化制备亚砜/砜  

Sulfoxide/sulfone preparation from selective oxidation of thioether promoted by mechanical forces

作　　者：王金龙 范吉霞 刘祈星 周海峰 WANG Jinlong;FAN Jixia;LIU Qixing;ZHOU Haifeng(Research Center of Green Pharmaceutical Technology and Process,Hubei Key Laboratory of Natural Products Research and Development,College of Biological and Pharmaceutical Sciences,China Three Gorges University,Yichang 443002,Hubei,China)

机构地区：[1]三峡大学生物与制药学院天然产物研究与利用湖北省重点实验室绿色制药技术与工艺研究中心,湖北宜昌443002

出　　处：《精细化工》2024年第11期2546-2552,共7页Fine Chemicals

基　　金：国家自然科学基金项目(22278244)。

摘　　要：以过氧硫酸氢钾复合盐(Oxone)为氧化剂,在室温、无溶剂球磨条件下,考察了二苯硫醚选择性氧化制备亚砜或砜的反应条件,并考察了底物的普适性。结果表明,在氧化剂Oxone用量1.0~4.0 mmol、160个氧化锆球(其中,直径为10、8、5 mm氧化锆球的数量比分别为20∶40∶100)、球磨时间5~50 min和转速400 r/min的条件下,硫醚类化合物实现了系列亚砜或砜类化合物的高选择性制备(收率90%~99%),产物通过^(1)HNMR、^(13)CNMR进行了确认。该法具有选择性好、收率高、底物适用范围广等优点。The reaction conditions for selective oxidation of diphenylene sulfide to sulfoxide or sulfone using potassium bisulfate complex salt(Oxone)as oxidant was investigated at room temperature under solvent-free ball milling conditions,followed by analysis on the universality of the substrate.The results showed that under the conditions of 1.0 to 4.0 mmol Oxone,160 zirconia balls(the number ratio of 10,8 and 5 mm zirconia balls was 20∶40∶100),5~50 min milling time and 400 r/min rotation speed,highly selective oxidation of thioether compounds to a series of sulfoxides or sulfones was achieved(yields 90%~99%),with the products confirmed by^(1)HNMR and^(13)CNMR.This method exhbited the advantages of good selectivity,high yield and wide application range of substrates.

关 键 词：机械化学 研磨法 砜 亚砜 选择性氧化 硫醚 

分 类 号：TQ227.2[化学工程—有机化工]