kmno4
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NaBPh4 from NaBF4 and PhMgBr
I'm looking for detailed information about synthetic procedure of preparation of NaBPh4:
NaBF4 + PhMgBr(or Cl) -> NaBPh4 (+ inorganic salts)
Unfortunately, all informations I can find lead to incorrect references. Strange....
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kristofvagyok
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| Quote: | 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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-found this in Tetrahedron, 2010 , vol. 66, # 38 p. 7633 - 7641
Also a similar producere with 80% yield in Bulletin of the Chemical Society of Japan Vol. 57 (1984) No. 9 P 2600-2604.
And it says that there is another recipe on similar ways in: Gmelin Handbook: Na: SVol.3, 4.3, page 1305 - 1312
[Edited on 25-5-2012 by kristofvagyok]
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kmno4
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Thanks.
Procedure from Tetrahedron is very similar to procedure from Analytica Chimica Acta, found earlier. Both procedures utilize very
large amounts of Et2O for few grams of product. I will see, if such large amouts are really needed.
In article from Bulletin of the Chemical Society of Japan, they use BF3 etherate , not NaBF4.
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