Department of Chemistry, Winston Salem State University, 601 S. Martin Luther King Jr. Dr., Winston Salem, NC 27110, USA.
Biomedical Research Infrastructure Center, Winston Salem State University, Winston Salem, NC 27110, USA.
Molecules. 2020 May 1;25(9):2128. doi: 10.3390/molecules25092128.
Grignard reagents undergo conjugate addition to thiochromones catalyzed by copper salts to afford 2-substituted-thiochroman-4-ones, both 2-alkylthiochroman-4-ones and thioflavanones (2-arylthiochroman-4-ones), in good yields with trimethylsilyl chloride (TMSCl) as an additive. The best yields of 1,4-adducts can be attained with CuCN∙2LiCl as the copper source. Excellent yields of 2-alkyl-substituted thiochroman-4-ones and thioflavanones (2-aryl substituted) are attained with a broad range of Grignard reagents. This approach works well with both alkyl and aromatic Grignard reagents, thus providing a unified synthetic approach to privileged 2-substituted thiochroman-4-ones and a potential valuable precursor for further synthetic applications towards many pharmaceutically active molecules. The use of commercially available and/or readily prepared Grignard reagents will expedite the synthesis of a large library of both 2-alkyl substituted thiochroman-4-ones and thioflavanones for additional synthetic applications.
格氏试剂在铜盐的催化下与硫色酮发生共轭加成反应,以三甲基氯硅烷(TMSCl)为添加剂,可得到 2-取代硫代色满-4-酮、2-烷基硫代色满-4-酮和硫色烷酮(2-芳基硫代色满-4-酮),产率良好。以 CuCN·2LiCl 作为铜源,可以获得最佳的 1,4-加成产物收率。Grignard 试剂具有广泛的范围,可以获得 2-取代的硫代色满-4-酮和硫色烷酮(2-芳基取代)的优异产率。该方法适用于烷基和芳基 Grignard 试剂,因此为受保护的 2-取代硫代色满-4-酮提供了一种统一的合成方法,并为进一步合成许多具有生物活性的分子提供了有价值的潜在前体。使用商业上可获得的和/或易于制备的 Grignard 试剂将加快 2-取代的硫代色满-4-酮和硫色烷酮的大型文库的合成,以进行更多的合成应用。