Mechanical activation of magnesium turnings for the preparation of reactive Grignard reagents
作者:Karen V. Baker、John M. Brown、Nigel Hughes、A. Jerome Skarnulis、Ann Sexton
DOI:10.1021/jo00002a039
日期:1991.1
Preactivation of magnesium by dry stirring in an inert atmosphere is highly beneficial for the clean synthesis of reactive allylic or benzylic organomagnesium chlorides. This procedure routinely produces 0.4 M solutions of the Grignard reagent in diethyl ether free from coupling products. The purity may be directly assayed by C-13 NMR spectroscopy. Using spin saturation transfer techniques, the rate constant for interconversion of the enantiomers of (1-phenyl-2-methylpropyl)magnesium chloride in Et2O at 25-degrees-C was shown to be < 0.2s-1. Electron microscopy has been used to define the surface changes occurring e during the dry stirring of magnesium turnings.
BAKER, KAREN V.;BROWN, JOHN M.;HUGHES, NIGEL;SKARNULIS, A. JEROME;SEXTON,+, J. ORG. CHEM., 56,(1991) N, C. 698-703
作者:BAKER, KAREN V.、BROWN, JOHN M.、HUGHES, NIGEL、SKARNULIS, A. JEROME、SEXTON,+