Process for separating mixtures of 3- and 4-nitrophthalic acid
AssigneeCiba-Geigy Corporation
InventorsPeter Furrer, Harry Beyeler
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AssigneeCiba-Geigy Corporation
InventorsPeter Furrer, Harry Beyeler
Estimating the term…
A novel improved process for separating mixtures of 3- and 4-nitrophthalic acid is described. The said process comprises treating a mixture of 3- and 4-nitrophthalic acid, which mixture is free from inorganic acid residues, in an aqueous-organic medium containing 1-20 percent by volume of water, at a temperature of between 20.degree. and 100.degree. C., stepwise with a base capable of forming salts of 3- and 4-nitrophthalic acid, which salts are essentially insoluble in the reaction medium, the treatment being carried out by adding base until a pH value of about 2.8 is obtained, separating the precipitating product consisting mainly of a 3-nitrophthalic acid mono-salt, subsequently precipitating, by the addition of further base, a product consisting principally of a 4-nitrophthalic acid salt, and finally converting the resulting nitrophthalic acid salts separately into the corresponding free acids, and optionally purifying these. The 3- and 4-nitrophthalic acid can be obtained by the process according to the invention in a simple manner in an isomer-free form and in good to very good yields.
A process for separating mixtures of 3- and 4-nitrophthalic acid, which process comprises treating a mixture of 3- and 4-nitrophthalic acid, which mixture is free from inorganic acid residues, in an aqueous-organic medium containing 1-20 percent by volume of water, at a temperature of between 20.degree. and 100.degree. C., stepwise with a base capable of forming salts of 3- and 4-nitrophthalic acid, which salts are essentially insoluble in the reaction medium, the treatment being carried out by adding base until a pH value of about 2.8 is obtained, separating the precipitating product consisting mainly of a 3-nitrophthalic acid mono-salt, subsequently precipitating, by the addition of further base, a product consisting principally of a 4-nitrophthalic acid salt, and finally converting the resulting nitrophthalic acid salts separately into the corresponding free acids.
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