Keck Gary E, Yu Tao, McLaws Mark D
Department of Chemistry, University of Utah, Salt Lake City, Utah 84112, USA.
J Org Chem. 2005 Apr 1;70(7):2543-50. doi: 10.1021/jo048308m.
[reaction: see text] Reactions of the bifunctional allylstannane 2-(chloromethyl)-3-(tributylstannyl)propene with aldehydes have been examined. These generally occur in high yields using Lewis acid promoters and the products can be isolated and purified without incident. Good yields and high enantioselectivities are also realized in catalytic asymmetric allylations (CAA reactions) using the previously described BITIP catalyst system. Protection of the free hydroxyl can be accomplished without cyclization to the derived tetrahydrofuran, although this transformation is also facile. The utility of the incorporated allyl chloride functionality allows for the obvious use of such products in reactions with nucleophiles. Use of these products in a less obvious connective strategy is demonstrated in the synthesis of the C12-C27 segment of bryostatin 1 where a connective, or "lynchpin", double-allylation process was employed. The beta-hydroxy allyl chloride obtained from an initial chelation-controlled allylation of aldehyde 16 was converted to allylstannane 19 and applied in a second allylation reaction, thus allowing for a highly convergent synthesis of the bryostatin C ring backbone in a stereoselective fashion.
[反应:见正文] 已研究了双官能团烯丙基锡烷2-(氯甲基)-3-(三丁基锡基)丙烯与醛的反应。使用路易斯酸促进剂时,这些反应通常产率很高,产物可以顺利分离和纯化。使用先前描述的BITIP催化剂体系进行催化不对称烯丙基化反应(CAA反应)时,也能实现良好的产率和高对映选择性。游离羟基的保护可以在不环化生成衍生四氢呋喃的情况下完成,尽管这种转化也很容易。引入的烯丙基氯官能团的实用性使得此类产物可明显用于与亲核试剂的反应。在苔藓抑素1的C12 - C27片段的合成中展示了这些产物在一种不太明显的连接策略中的应用,其中采用了一种连接性的或“关键”的双烯丙基化过程。从醛16的初始螯合控制烯丙基化反应得到的β - 羟基烯丙基氯转化为烯丙基锡烷19,并应用于第二次烯丙基化反应,从而以立体选择性方式实现了苔藓抑素C环骨架的高度汇聚合成。