Large-scale preparation and labelling reactions of deuterated silanes

作者:Campos Jesus; Rubio Miguel; Esqueda Ana C; Carmona Ernesto*
来源:Journal of Labelled Compounds and Radiopharmaceuticals, 2012, 55(1): 29-38.
DOI:10.1002/jlcr.1950

摘要

A catalytic synthesis of deuterated silanes SiEt3D, SiMe2PhD and SiPh2D2 is reported that allows their facile generation in a 3-4 g scale, utilizing D2 (0.5 bar) as the hydrogen isotope source and low catalyst loadings (0.01 mol%). The catalyst precursor is the rhodium (III) complex 1, which contains a (eta 5-C5Me5)Rh cation stabilized by coordination to a cyclometallated phoshine PMeXyl2 (Xyl=2,6-C6H3Me2). The same complex is also an active catalyst for the hydrosilylation of the C=O and C=N bonds of various ketones, aldehydes and alpha,beta-unsaturated nitriles. Hence, combination of these two properties permits development of a simple and proficient one-flask, two-step procedure for the deuterosilylation of these substrates.

  • 出版日期2012-1