Typical experimental procedure for the synthesis of NaBAr4
Slow addition of a solution of (0.09 mol) of aryl bromides in Et2O (150 mL) to Mg turnings (0.11 mol) in Et2O (150 mL), followed by refluxing for 30
min, gave a dark gray solution of the aryl Grignard reagent. Upon addition of NaBF4 (0.15 mol), the heterogeneous reaction mixture was stirred for 48
h, during which time the solution became brown and a fine precipitate formed. The reaction mixture was then added to Na2CO3 (38 g) in water (1 L),
stirred for 20 min, and then filtered. The mixture was extracted with Et2O (4×100 mL) and the combined organic layer was dried over Na2SO4 and
concentrated in vacuo. The residue was recrystallized from petroleum ether.
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