Perfluoroalkyl Grignard Reagents: NMR Study of 1-Heptafluoropropylmagnesium Chloride in Solution.
We report on the generation of a perfluoroalkyl Grignard reagent ((F)RMgX) by exchange reaction between a perfluoroalkyl iodide ((F)R-I) and a Grignard reagent (RMgX). (19)F NMR was applied to monitor the generation of n-C3F7MgCl. Additional NMR techniques, including (19)F COSY, NOESY, and pulsed gradient spin-echo (PGSE) diffusion NMR, were invoked to assign peaks observed in (19)F spectrum. Schlenk equilibrium was observed and was significantly influenced by solvent, diethyl ether, or THF.
Department of Chemistry, Brown University , Providence, Rhode Island 02912, United States.
Jie
J
Guang
Department of Chemistry, Brown University , Providence, Rhode Island 02912, United States.
Russell
R
Hopson
Department of Chemistry, Brown University , Providence, Rhode Island 02912, United States.
Paul G
PG
Williard
Department of Applied Chemistry, Tokyo Institute of Technology , Tokyo 152-8552, Japan.
Motohiro
M
Fujiu
Department of Applied Chemistry, Tokyo Institute of Technology , Tokyo 152-8552, Japan.
Kazuyuki
K
Negishi
Department of Applied Chemistry, Tokyo Institute of Technology , Tokyo 152-8552, Japan.
Koichi
K
Mikami