Jezorek Ryan L, Zhang Na, Leowanawat Pawaret, Bunner Matthew H, Gutsche Nicholas, Pesti Aleksander K R, Olsen James T, Percec Virgil
Roy & Diana Vagelos Laboratories, Department of Chemistry, University of Pennsylvania , Philadelphia, Pennsylvania 19104-6323, United States.
Org Lett. 2014 Dec 19;16(24):6326-9. doi: 10.1021/ol503061c. Epub 2014 Dec 3.
A library containing 10 air-stable Ni(II)X(Aryl)(PCy3)2 σ-complexes as precatalysts (X = Cl, Br, OTs, OMs, aryl = 1-naphthyl, 2-naphthyl; X = Cl, 1-acenaphthenyl, 1-(2-methoxynaphthyl), 9-phenanthrenyl, 9-anthracyl) was synthesized and demonstrated to quantitatively cross-couple 2-methoxyphenyl dimethylsulfamate with methyl 4-(5,5-dimethyl-1,3,2-dioxaborinane-2-yl)benzoate at 23 °C in dry THF in the presence of K3PO4(H2O)3.2 in less than 60 min. Lower or higher amounts of H2O in K3PO4 and as received THF mediate the same transformation in a maximum three times longer reaction time.
合成了一个包含10种空气稳定的Ni(II)X(芳基)(PCy3)2 σ-配合物作为预催化剂的文库（X = Cl、Br、OTs、OMs，芳基 = 1-萘基、2-萘基；X = Cl、1-苊烯基、1-(2-甲氧基萘基)、9-菲基、9-蒽基），并证明在23℃下，在干燥四氢呋喃中，在K3PO4(H2O)3.2存在下，该文库能在不到60分钟的时间内使2-甲氧基苯基二甲基氨基磺酸酯与4-(5,5-二甲基-1,3,2-二氧硼杂环戊烷-2-基)苯甲酸甲酯进行定量交叉偶联反应。K3PO4中较低或较高含量的水以及所使用的四氢呋喃会使相同的转化反应时间最长延长三倍。
