Paterson Ian, Housden Michael P, Cordier Christopher J, Burton Paul M, Mühlthau Friedrich A, Loiseleur Olivier
University Chemical Laboratory, Lensfield Road, Cambridge, CB2 1EW, UK.
Org Biomol Chem. 2015 May 28;13(20):5716-33. doi: 10.1039/c5ob00498e. Epub 2015 Apr 22.
The brasilinolides are an architecturally complex family of 32-membered macrolides, characterised by potent immunosuppressant and antifungal properties, which represent challenging synthetic targets. By adopting a highly convergent strategy, a range of asymmetric aldol/reduction sequences and catalytic protocols were employed to assemble a series of increasingly elaborate fragments. The controlled preparation of suitable C1-C19 and C20-C38 acyclic fragments 5 and 6, containing seven and 12 stereocentres respectively, was first achieved. An adventurous C19-C20 fragment union was then explored to construct the entire carbon chain of the brasilinolides. This pivotal coupling step could be performed in a complex boron-mediated aldol reaction to install the required C19 hydroxyl stereocentre when alternative Mukaiyama-type aldol protocols proved unrewarding. A protected C1-C38 polyol 93 was subsequently prepared, setting the stage for future late-stage diversification toward the various brasilinolide congeners. Throughout this work, asymmetric boron-mediated aldol reactions of chiral ketones with aldehydes proved effective both for controlled fragment assembly and coupling with predictable stereoinduction from the enolate component.
巴西内酯是一类结构复杂的32元大环内酯类化合物,具有强大的免疫抑制和抗真菌特性,是具有挑战性的合成目标。通过采用高度汇聚的策略,一系列不对称羟醛缩合/还原序列和催化方法被用于组装一系列日益复杂的片段。首先实现了分别含有7个和12个立体中心的合适的C1-C19和C20-C38无环片段5和6的可控制备。然后探索了一个大胆的C19-C20片段连接,以构建巴西内酯的整个碳链。当替代的 Mukaiyama 型羟醛缩合方法被证明无效时,这个关键的偶联步骤可以在一个复杂的硼介导的羟醛缩合反应中进行,以安装所需的C19羟基立体中心。随后制备了一个受保护的C1-C38多元醇93,为未来向各种巴西内酯类似物的后期多样化奠定了基础。在整个这项工作中,手性酮与醛的不对称硼介导的羟醛缩合反应被证明对于可控的片段组装以及与烯醇盐组分可预测的立体诱导偶联都是有效的。