The method of obtaining piperazine-adipate

 

(57) Abstract:

The invention relates to the field of chemistry, to a method for the chemical substance that manifests anthelminthic properties, and can be used in agriculture to treat animals. The aim of the invention is to simplify the process technology. The process is suggested by the interaction hexahydropyrazino with adipic acid in the solid phase under stirring at a temperature of 20-25oC at a molar ratio of 1:1 to achieve the reaction mass pH 6-7 and subsequent distillation of the liberated in the reaction of water and drying of the target product.

The invention relates to a method for producing piperazine-adipate, which is an anthelmintic drug used to treat animals.

Known method (patent Poland 56 135) obtain piperazine-adipate, which consists in the interaction piperazine-uranyl and adipic acid in the aquatic environment:

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The reaction is carried out as follows.

130 kg (0,89 g-mol) of adipic acid are dissolved at 70-80oC 300 kg (16,67 g-mol) of distilled water, then add 1 kg of activated carbon, and conducting filtering piperazine - 0,89 g-mol) in 80 kg of distilled water with a temperature of 70oC to establish pH 6-7,5. The molar ratio of adipic acid piperazine 1 1. The mixture is distilled in a vacuum to 240 kg of water, the residue is cooled to 18oC and filtered. The precipitate is washed with a small amount of distilled water and dried at 60oC. the mother liquor is diluted with water to a total volume of 400 l and used for dissolving the following portions of adipic acid. After several cycles the mother liquor is evaporated to 4/5 and after recrystallization from water (mass ratio of water piperazine-adipate 7 1) allocate an additional amount of piperazine-adipate. The total yield of 95-96% (based on adipic acid.

The disadvantage of this method is the complexity of the technological process, based on: 1) the need for pre-cleaning of adipic acid; 2) the use of scarce activated carbon for the purification of acid; 3) the disposal of large quantities of waste water; 4) the presence of various equipment (reactor, filter, refrigerator, collection and others) to build the process flowsheet.

The aim of the invention is the simplification of the process of obtaining piperazine-adipate.

Supplied with the x mark PLN or drier "Violet". The mixing is carried out at a temperature of 20-25oC for 1.5-2 h, the molar ratio of components 1 1. It releases water of crystallization and is formed piperazine-adipate in paste form. If 70oC, vacuum and continuously operating the agitator is stripped separated from the reaction of water for 2-3 hours Following example illustrates the method of obtaining piperazine-adipate.

Example.

In mixer brand PLN or drier "Violet" download at 20-25oC g (2.65 g-mol) piperazine-uranyl and 386,9 g (2.65 g-mol) of adipic acid and stirred at this temperature for 1.5-2 h, forming a paste with a pH of aqueous paste 6-6,1. Then to the mixer or dryer hook up the vacuum, heated to 60-90oC and distilled water with the receiving water in the sink for 2-2,5 hours Get 605,9 g dry piperazine-adipate, a yield of 99%

Thus, the proposed method can greatly simplify the process of obtaining piperazine-adipate due to:

1) the reaction product education and drying in a single unit, eliminating a number of equipment;

2) reduction of wastewater, because the mixing of the reagents is carried out in the solid phase in the absence of solvent.

the s reagent ratio 1 1, characterized in that the interaction is carried out in the apparatus mixers brand PLN or drier "Violet" in the solid phase at 20 25oC and stirring, followed by distillation of the reaction water at 70 to 80oWith the vacuum.

 

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