METHOD FOR PRODUCING A MIXTURE OF MONO-, DI-, TRI-TERT-BUTYLFERROCENES Russian patent published in 2022 - IPC C07F17/02 B01J31/22 

FIELD: tert-butylferrocene production.

SUBSTANCE: invention relates to a method for producing tert-butylferrocene in the form of a mixture of mono-, di-, tri-tert-butylferrocenes used as a plasticizer-combustion catalyst. The method includes mixing ferrocene with alkyl halide, such as tert-butyl chloride, in an organic solvent - dichloroethane in the presence of a catalyst - aluminum chloride, holding the reaction mass, decomposition of the catalyst, separation of the solvent and subsequent isolation of the finished product. At the same time, the catalyst is preliminarily prepared by adding dry ferrocene and anhydrous aluminum chloride to the solvent - dichloroethane at a molar ratio of ferrocene: aluminum chloride: dichloroethane equal to 1:1:23.4 with stirring at a temperature of 0-2°C until complete dissolution of aluminum chloride, obtaining homogeneous activated catalytic complex. Next, tert-butyl chloride is dosed into the prepared catalytic complex at a temperature of 0-25°C. The molar ratio of ferrocene: aluminum chloride : tert-butyl chloride : dichloroethane is 1:1:(1.2-1.49):23.4. The finished product is isolated by fractional vacuum distillation at a temperature in vapors of 125-145°C at 3-4 mm Hg. in the form of a mixture of tert-butylferrocenes containing mono- not less than 60 wt.%, di-25-35 wt.%, tri-tert-butylferrocene no more than 5 wt.% and unreacted ferrocene no more than 5 wt.%.

EFFECT: proposed method allows to increase the conversion of ferrocene up to 93-95% and the product yield up to 82-87% based on the reacted ferrocene.

2 cl, 3 ex