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4-(tert-Butyldimethylsiloxy)phenylmagnesium bromide, 0.50 M in THF synthesis

1synthesis methods
-

Yield:-

Reaction Conditions:

iodine in tetrahydrofuran at 25 - 60;

Steps:

1.2.B

B. Grignard derivative of the protected 4 -Bromophenol (4); The silylated aryl bromide (3) (3.62 g, 12.6 mmol) was added to magnesium (306 mg, 12.6 mmol, 1 .0 equiv) in 30 mL of dry THF under nitrogen in the presence of a catalytic amount of iodine at 60 0C. After the red brown color of the mixture disappeared, the reaction mixture was cooled to 25°C and stirred until the magnesium was almost consumed (2 - 5 hours).

References:

WO2009/80796,2009,A1 Location in patent:Page/Page column 15; 17