Organic compounds -- part of the class 532-570 series – Organic compounds – Heterocyclic carbon compounds containing a hetero ring...
Patent
1985-08-26
1987-02-10
Daus, Donald G.
Organic compounds -- part of the class 532-570 series
Organic compounds
Heterocyclic carbon compounds containing a hetero ring...
C07D20948
Patent
active
046423540
DESCRIPTION:
BRIEF SUMMARY
FIELD OF THE ART
The present invention relates to the organic synthesis of and, more particularly, to a process for producing phthalimides of alkali metals.
DESCRIPTION OF THE PRIOR ART
Known in the art is a process for producing potassium phthalimide by reacting a 5% solution of phthalimide in absolute ethanol with a 25% ethanolic solution of potassium hydroxide. After decanting the solutions the reaction mass is rapidly cooled, filtered-off to remove the formed potassium phthalimide, the precipitate is then suspended in acetone, filtered and dried in air with moderate heating to give about 90% of the product (Experimental Methods in Organic Chemistry, Moscow, "Khimiya" Publishing House, 1969, p. 415).
This prior art process features a low yield of the desired product, a considerable rate of consumption of ethanol and acetone; the process is also characterized by the use of explosive and flammable solvents.
Also known in the art is a process for the production of phthalimides of alkali metals by reacting a suspension of a finely-divided phthalimide in dehydrated aliphatic alcohols containing 1 to 4 carbon atoms in a molecule with a solution of an alkali metal hydroxide or alcoholate in the same alcohols. The process is conducted at a temperature within the range of from 35.degree. to 50.degree. C. for a period of 1 to 6 hours. After residence for a certain period the suspension is cooled to 20.degree. C., the precipitate is washed with alcohol and dried. The yield of the desired product is 85% (cf. British Pat. No. 1,420,523 Cl. C 2 C, published 1976).
As can be seen, this process also features a low yield of the desired product. Also known is a process for producing phthalimides of alkali metals, consisting of adding a mixture of solutions of an alkali metal butylate and hydroxide in an organic solvent in a molar ratio of the alkali metal butylate to the alkali metal hydroxide equal to 0.5:0.5-0.99:0.01 by metering to a suspension of phthalimide in an organic solvent at a temperature of from 50.degree. to 110.degree. C. for 60-70 minutes. The synthesis is carried out in a vessel provided with a stirrer and a reflux condenser to recycle the solvent vapours. After complete intermixing of the reactants the reaction mass is kept for 20 minutes, cooled, filtered, and dried. To prepare a suspension of phthalimide, butanol, benzene, chlorobenzene, or white-spirit is used as an organic solvent. For the preparation of a solution of an alkali metal butylate or alkali metal hydroxide, butanol or its mixture with the above-mentioned solvents is used. The product yield is equal to 97-99%, the content of the main substance is 95-99% (cf. USSR Inventor's Certificate No. 875794, Int. Cl. C 07 D 209/48, published 1982).
This process features rather complicated and lasting auxiliary stages of filtration and drying of the product to remove the organic solvent. The suspension of the product, obtained in the above-described manner, is unsatisfactorily filtered, the precipitate is unsatisfactorily pressed and, hence, contains a considerable percentage (50-70%) of the solvent. The filtered-off cake is liable to a thixotropic liquefaction under the effect of mechanical loads; it adheres to metal surfaces, thus appreciably hindering transportation of the slurry from the filter to the drier. The adherence of the product to the walls and rotor of the vacuum-scraper drier complicates the drying process, makes it time consuming and less effective. The duration of the drying stage is 5-6 hours, and that of the entire process is 6.5 to 8.5 hours.
DESCRIPTION OF THE INVENTION
It is an object of the present invention to provide such a process for producing phthalimides of alkali metals, which would be more simple in practical implementation.
This object is accomplished by the production of phthalimides of alkali metals by way of interaction of a phthalimide with an alcoholic solution of an alkali metal hydroxide and/or an alkali metal alcoholate at a temperature within the range of from 50.degree. to 100.degree. C. In accordance
REFERENCES:
N. N. Suvorov (ed.), Weigand-Hilgetag, Experimental Methods in Organic Chstry (translation from 3-d German edition), Moscow, "Khimiya" publishers, p. 415 (1968).
Davituliani Valentin V.
Dudin Vladimir P.
Gorbunov Boris N.
Khlybov Vyacheslav I.
Konov Vyacheslav V.
Ceperley Mary E.
Daus Donald G.
Nauchno-Issledovatelsky Institut Khimikatov Dlya Polimernykh Mat
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