Process for the preparation of pivaloyl cyanide

Details Process for the preparation of pivaloyl cyanide Process for the preparation of pivaloyl cyanide

B - Operations, Transporting

01

J

260/561.9

B01J 31/16 (2006.01)

Patent

CA 1165778

ABSTRACT OF THE DISCLOSURE In the preparation of pivaloyl cyanide of the formula (CH3)3C-CO-CN by reaction of pivalic acid anhydride with anhydrous hydrocyanic acid, the improvement which comprises carrying out the reaction continuously in the presence of a catalyst comprising an alkali metal/copper cyanide complex, an alkaline earth metal/copper cyanide complex or an alkali metal salt, or an alkaline earth metal salt, of an aliphatic, cycloalkphatic or aromatic, carboxylic acid, or a precursor of such a salt, in either case optionally in admixture with a Lewis acid, and in the presence of an inert, aprotic organic diluent, which boils above about 210°C, at a temperature between about 180° and 240°C, by simultaneously and continuously dropping the pivalic acid anhydride and introducing the hydrocyanic acid in gaseous form into a stirred suspension of the catalyst in the diluent, and continuously distilling the crude product mixture consisting essentially of pivaloyl cyanide, pivalic acid and unreacted hydrocyanic acid, the unreacted hydro- cyanic acid being separated off by evaporation and being recycled to the reaction vessel, and the pivaloyl cyanide being separated from the precipitated crude product mix- ture by fractional distillation in vacuo. Advantageously the reaction is carried out at a temperature between about 195° and 225°C, the complex cyanide of the formula Ma3[Cu(CN)4], K3[Cu(CN)4], Ca3[Cu(CN)4]2 or Ba3[Cu(CN)4]2 is employed as the catalyst, diphenyl ether is employed as the diluent, and about 1 to 2 moles of pivalic acid anhydride and about 5 to 8 moles of hydrocyanic acid are introduced into the suspension of catalyst per hour. Le A 20 711

391216

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