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ChemicalBook CAS DataBase List Di-n-butylmagnesium

Di-n-butylmagnesium synthesis

10synthesis methods
-

Yield:1191-47-5 80%

Reaction Conditions:

with magnesium in diethyl ether at 40; for 4 h;Inert atmosphere;

Steps:

A1 (Synthesis of dibutyl magnesium)

Under argon atmosphere, into a 100 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 5.5 g (0.23 mol) of metallic magnesium and 20 ml of diethyl ether.
And then, 3.0 g (21 mmol) of bromobutane was slowly dropped into the flask.
Subsequently, 180 ml of diethyl ether and 25 g (0.18 mol) of bromobutane were slowly dropped into the flask, and the mixture was reacted while stirring at 40 °C for 2 hours.
And then, 55 g (0.62 mol) of dioxane was added to the reaction solution, and the mixture was reacted while stirring at 40 °C for 2 hours.
After the completion of the reaction, under argon atmosphere, the reaction solution was filtrated, and the filtrate was concentrated under reduced pressure.
The resultant concentrate was heated and dried under vacuum, to provide 22 g of dibutyl magnesium. (Isolation yield: 80 %)

References:

EP2636674,2013,A1 Location in patent:Paragraph 0139

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