Abstract:
1,125,158. Carbonylation of unsaturated compounds. BADISCHE ANILIN- & SODAFABRIK A.G. 17 Dec., 1965 [19 Dec., 1964], No. 53574/65. Heading C2C. In a process for preparing carboxylic acids, esters or halides by reacting olefinically unsaturated compounds with carbon monoxide and water, or alcohol, or phenol, or a halogen halide, or by reacting acetylenically unsaturated compounds with carbon monoxide and a hydrogen halide, at elevated temperature and superatmospheric pressure in the presence of a palladium catalyst, the catalyst reused may be a solution obtained from the residue of the distillation and/or extraction of the acid constituents by alkaline reacting substances, of the reaction mixture, to which is added an organic phosphine. Phosphines mentioned are triarylphosphines and tricycloalkylphosphines. Examples describe the preparation of cyclododecadiene-(5,9) - carboxylic - (1) - carboxylic acid and the methyl and ethyl esters thereof and propionyl chloride in which the palladium catalyst is reused with the addition of organic phosphine.
Abstract:
A process for the recovery of methylglyoxal acetal from a reaction mixture which has been obtained in the reaction of acetone with an alcohol and a nitrosation agent or oxidizing agent in the presence of an acid catalyst followed by neutralization which comprises diluting the neutralized reaction mixture with such an amount of water that a homogeneous solution is formed, subsequent distillation in a first column in which a mixture of acetone, alcohol and solvent is removed overhead and returned direct to the synthesis and an azeotrope of methylglyoxal acetal, water and high-boilers is withdrawn as a side stream, condensation of the azeotrope thus obtained and separation of the phase rich in methylglyoxal acetal, subsequent distillation of the phase rich in methylglyoxal acetal thus obtained in a second column in which purified methylglyoxal acetal is withdrawn as a side stream and the overhead and bottoms products are returned with the feed to the first column, pure methylglyoxal acetal being obtained as the overhead product in a third column. Methylglyoxal acetal is suitable for the production of animal feed supplements.