Liu Wei, Ding Decai, Yin Lingfeng, Poore Andrew, Ho Yeu-Shiuan, Cheng Yu-Ho, Hsieh Chi-Tien, Yachuw Stephen, Knieser Rachael, Krause Jeanette, Tian Shiliang, Cheng Mu-Jeng
Res Sq. 2024 Aug 16:rs.3.rs-3645899. doi: 10.21203/rs.3.rs-3645899/v1.
Stereochemical-controlled hydrogen bond donors play essential roles in the pharmaceutical industry. Consequently, organic molecules that bear difluoromethyl (CF2H) groups at chiral centers are emerging as pivotal components in pharmaceuticals due to their distinct hydrogenbonding property. However, a general approach for introducing CF2H groups in an enantioselective manner remained elusive. Here, we show that enantioconvergent difluoromethylation of racemic alkyl electrophiles, through alkyl radical intermediates, represents a new strategy for constructing CF2H-containing stereocenters. This strategy is enabled by using copper catalysts bound with a chiral diamine ligand bearing electron-deficient phenyl groups, and a nucleophilic difluoromethyl-zinc reagent. This method allows for the high-yield conversion of a diverse range of alkyl halides into their alkyl-CF2H analogs with excellent enantioselectivity (up to 99% e.e.). Mechanistic studies, supported by DFT calculations, revealed a route involving asymmetric difluoromethylation of alkyl radicals and crucial non-covalent interactions in the enantio-determining steps.
立体化学控制的氢键供体在制药工业中起着至关重要的作用。因此,在手性中心带有二氟甲基(CF2H)基团的有机分子因其独特的氢键性质而成为药物中的关键成分。然而,以对映选择性方式引入CF2H基团的通用方法仍然难以捉摸。在这里,我们表明,通过烷基自由基中间体对外消旋烷基亲电试剂进行对映汇聚式二氟甲基化,代表了一种构建含CF2H立体中心的新策略。该策略通过使用与带有缺电子苯基的手性二胺配体结合的铜催化剂和亲核二氟甲基锌试剂得以实现。该方法能够将多种卤代烷高效转化为其烷基-CF2H类似物,对映选择性优异(高达99% ee)。在DFT计算支持下的机理研究揭示了一条涉及烷基自由基的不对称二氟甲基化以及对映决定步骤中关键非共价相互作用的途径。