Department of Chemistry, Merkert Chemistry Center, Boston College , Chestnut Hill, Massachusetts 02467, United States.
J Am Chem Soc. 2017 Jul 5;139(26):9053-9065. doi: 10.1021/jacs.7b05011. Epub 2017 Jun 24.
A practical method for enantioselective synthesis of fluoroalkyl-substituted Z-homoallylic tertiary alcohols has been developed. Reactions may be performed with ketones containing a polylfluoro-, trifluoro-, difluoro-, and monofluoroalkyl group along with an aryl, a heteroaryl, an alkenyl, an alkynyl, or an alkyl substituent. Readily accessible unsaturated organoboron compounds serve as reagents. Transformations were performed with 0.5-2.5 mol % of a boron-based catalyst, generated in situ from a readily accessible valine-derived aminophenol and a Z- or an E-γ-substituted boronic acid pinacol ester. With a Z organoboron reagent, additions to trifluoromethyl and polyfluoroalkyl ketones proceeded in 80-98% yield, 97:3 to >98:2 α:γ selectivity, >95:5 Z:E selectivity, and 81:19 to >99:1 enantiomeric ratio. In notable contrast to reactions with unsubstituted allylboronic acid pinacol ester, additions to ketones with a mono- or a difluoromethyl group were highly enantioselective as well. Transformations were similarly efficient and α- and Z-selective when an E-allylboronate compound was used, but enantioselectivities were lower. In certain cases, the opposite enantiomer was favored (up to 4:96 er). With a racemic allylboronate reagent that contains an allylic stereogenic center, additions were exceptionally α-selective, affording products expected from γ-addition of a crotylboron compound, in up to 97% yield, 88:12 diastereomeric ratio, and 94:6 enantiomeric ratio. Utility is highlighted by gram-scale preparation of representative products through transformations that were performed without exclusion of air or moisture and through applications in stereoselective olefin metathesis where Z-alkene substrates are required. Mechanistic investigations aided by computational (DFT) studies and offer insight into different selectivity profiles.
一种用于氟烷基取代 Z-高烯丙基叔醇对映选择性合成的实用方法已经开发出来。该反应可以用含有多氟、三氟、二氟和单氟烷基以及芳基、杂芳基、烯基、炔基或烷基取代基的酮进行。易于获得的不饱和有机硼化合物可用作试剂。转化在 0.5-2.5mol%的基于硼的催化剂存在下进行,该催化剂由易得的缬氨酸衍生的氨基酚和 Z-或 E-γ-取代的硼酸频哪醇酯原位生成。用 Z 型有机硼试剂,三氟甲基和多氟烷基酮的加成收率为 80-98%,α:γ 选择性为 97:3 至>98:2,>95:5 Z:E 选择性,81:19 至>99:1 对映体过量。与未取代的烯丙基硼酸频哪醇酯的反应形成鲜明对比的是,单氟或二氟甲基取代的酮的加成反应也具有高度对映选择性。当使用 E-烯丙基硼酸盐化合物时,转化同样高效且具有α和 Z 选择性,但对映选择性较低。在某些情况下,对映体相反(高达 4:96er)。用含有烯丙基手性中心的外消旋烯丙基硼酸盐试剂,加成反应具有非常高的α选择性,以高达 97%的收率、88:12 的非对映体比例和 94:6 的对映体过量,得到预期的来源于 crotylboron 化合物的γ加成产物。通过在不排除空气或水分的情况下进行的转化以及在需要 Z-烯烃底物的立体选择性烯烃复分解反应中的应用,突出了其实用性。由计算(DFT)研究辅助的机理研究提供了对不同选择性的深入了解。