Synthesis of Mg(BHT)2(THF)2
AssigneeThe University of Akron
InventorsMatthew Becker, Alex P. Kleinfehn, Shannon R. Petersen
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Abstract
In one or more embodiments, the present invention is directed to a novel method for synthesizing Mg(BHT)2(THF)2 catalyst, which has several advantages over previous methods. Dry toluene or pentane are not required for synthesizing the catalyst, and the reaction is done in a bulk solution of BHT and THF. Further, because the Mg(BHT)2(THF)2 is made in a one-step (“one-pot”) synthesis, the time required for synthesizing and drying the catalyst is reduced. Using the new method of the present invention, the Mg(BHT)2(THF)2 is pure after removing excess THF, thereby eliminating the need for washes and recrystallization.
Claims17
A method for making a magnesium 2,6-di-tert-butyl-4-methylphenoxide·tetrahydrofuran (Mg(BHT)2(THF)2) catalyst comprising:
- A) dissolving di-n-butylmagnesium in a suitable solvent to form a di-n-butylmagnesium solution;
- B) dissolving 2,6,di-tert-butyl-4-methylphenol in anhydrous tetrahydrofuran (THF) to form a 2,6,di-tert-butyl-4-methylphenol/THF solution;
- and
- C) adding the di-n-butylmagnesium solution to said 2,6,di-tert-butyl-4-methylphenol/THF solution;
- wherein said di-n-butylmagnesium reacts with said 2,6,di-tert-butyl-4-methylphenol and THF to form the Mg(BHT)2(THF)2 catalyst,
- wherein the yield of said Mg(BHT)2(THF)2 catalyst is 93% or greater by weight and the purity of said Mg(BHT)2(THF)2 catalyst is 98% or more without recrystallization.
A one pot method for making a magnesium catalyst comprising:
- A) reacting di-n-butylmagnesium, a 2,6,di-tert-butyl-4-methylphenol solution, and anhydrous tetrahydrofuran (THF) at ambient temperature over a water bath, ice bath, or heat sink to form magnesium 2,6-di-tert-butyl-4-methylphenoxide· tetrahydrofuran (Mg(BHT)2(THF)2) catalyst;
- and
- B) removing any remaining THF and solvent to produce a Mg(BHT)2(THF)2 catalyst with a_yield of said Mg(BHT)2(THF)2 catalyst of a 93% or greater by weight and a purity of 98% or more without recrystallization.
A method for making magnesium 2,6-di-tert-butyl-4-methylphenoxide·tetrahydrofuran (Mg(BHT)2(THF)2) catalyst comprising:
- A) dissolving di-n-butylmagnesium in hexane, heptane, or octane to form a 1M di-n-butylmagnesium solution;
- B) dissolving 2,6,di-tert-butyl-4-methylphenol in anhydrous tetrahydrofuran (THF) to form a 2,6,di-tert-butyl-4-methylphenol/THF solution;
- C) combining said di-n-butylmagnesium solution of Step A and said 2,6,di-tert-butyl-4-methylphenol/THF solution of Step B at a molar ratio of di-n-butylmagnesium to 2,6,di-tert-butyl-4-methylphenol of from about 1:2 to about 1:2.05 by adding the di-n-butylmagnesium solution of step A dropwise to the 2,6,di-tert-butyl-4-methylphenol/THF solution of step B over a water bath, ice bath, or heat sink at ambient temperature to form a Mg(BHT)2(THF)2 catalyst;
- D) stirring or agitating the combination of step C for from about 90 min to about 210 min or until substantially all of the di-n-butylmagnesium and 2,6,di-tert-butyl-4-methylphenol have reacted with THF to form the Mg(BHT)2(THF)2 catalyst;
- and
- E) removing any unreacted THF and solvent by evaporation under reduced pressure or rotary evaporation to produce the Mg(BHT)2(THF)2 catalyst, wherein the yield of said Mg(BHT)2(THF)2 catalyst is 93% or greater by weight and the purity of said Mg(BHT)2(THF)2 catalyst is 98% or more without recrystallization.
Dependencies are inferred from the claim text.