Shanghai Key Laboratory of Chemical Biology, School of Pharmacy, East China University of Science and Technology, Shanghai, 200237, China.
Mol Divers. 2011 Feb;15(1):109-13. doi: 10.1007/s11030-010-9261-6. Epub 2010 Oct 6.
The methodology of using a silica gel-supported functionalized ionic liquid as a scavenger in the purification of parallel synthesis products was demonstrated. Silica-supported sulfonic acid-functional ionic liquid was synthesized by etherification, aminate, and quaternary aminate from activated silica gel and 3-chloropropyl trimethoxysilane, imidazole, and 1,4-butanesultone, which was followed by acidification using trifluoromethanesulfonic acid and anion exchange with potassium hexafluorophosphate. A conventional ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate was then used to coat the surface of the silica gel. The silica-supported functionalized ionic liquid was used as a scavenger in the removal of excess amine in the parallel synthesis of amides. Desired products were obtained in excellent yields and purity with a sequestration time of less than 100 min at room temperature. After scavenging, the scavenger was easily filtered out and regenerated.
采用硅胶负载功能化离子液体作为净化平行合成产物的清除剂的方法得到了证明。硅胶负载磺酸基功能化离子液体通过醚化、氨化和季铵化反应，由活化硅胶和 3-氯丙基三甲氧基硅烷、咪唑和 1,4-丁烷砜合成，然后用三氟甲磺酸酸化并用六氟磷酸钾进行阴离子交换。然后使用常规离子液体 1-丁基-3-甲基咪唑六氟磷酸盐涂覆硅胶表面。硅胶负载功能化离子液体作为清除剂，用于去除酰胺平行合成中过量的胺。在室温下，不到 100 分钟的封闭时间即可获得收率和纯度优异的所需产物。清除后，清除剂很容易过滤并再生。
