Example 15
(1) Synthesis of a Magnesium Salt
Under argon gas atmosphere, diphenylsilanediol (8.65 g, 40 mmol) (Tokyo Chemical Industry Co., Ltd.) was dissolved in tetrahydrofuran (THF) (20 mL) (Wako Pure Chemical Industries, Ltd.), and then a THF solution of phenylmagnesium chloride (PhMgCl) (40 mL, 80 mmol) (Tokyo Chemical Industry Co., Ltd., 2 M) was added dropwise, and the solution was stirred for 1 hour. After that, powder generated by concentration and drying of the solution, was washed with diisopropyl ether (50 mL) (Wako Pure Chemical Industries, Ltd.). The powder was filtered off and dried to obtain diphenylsilanedioxy bis(magnesium chloride), (Ph2Si(OMgCl)2).
Measurement result of 1H-NMR is shown below.
1H-NMR (400 MHz, CDCl3) δ (ppm): 6.90-8.00 (m, 10H)
(2) Preparation of the Electrolytic Solution
Under argon gas atmosphere, into diphenylsilanedioxy bis(magnesium chloride) (Ph2Si(OMgCl)2) (0.83 g, 2.5 mmol), THF (20 mL) (Wako Pure Chemical Industries, Ltd.) was mixed. The mixture was heated to 50° C., and then aluminum chloride (AlCl3) (0.67 g, 5 mmol) (Wako Pure Chemical Industries, Ltd.) was added to the mixture. After maintaining the resulting mixture at 50° C. for 10 minutes, it was cooled to obtain the electrolytic solution 14, “a solution of diphenylsilanedioxy bis(magnesium chloride)-aluminum chloride/THF”.