The way to obtain 2,6-dimethyl-3,5-dichloro-4(1h)-pyridone

 

(57) Abstract:

Usage: for the treatment and prevention of coccidiosis in commercial poultry production. The inventive 2,6-dimethyl-3,5-dichloropyridine-4. Reagent 1: 2,6-dimethyl-4(14)pyridone. Reagent 2: sodium chloride. Reaction conditions: by electrolysis in a membrane electrolyzer on ksirodarnavasambhavam the anode when the anode current density 15-20 A/l, a temperature of 15-20 degrees.C and pH = 9, the concentration of reagent 1 5-20 g/l, and reagent 2 200-300 g/l, measured flow in the anode electrolyte reagents and aqueous solution of NaOH or Na2CO3. table 2., 1 Il.

The invention relates to chemical technology for veterinary drug 2,6-dimethyl-3,5-dichloro-4(1H) pyridone (tarmacced) used for treatment and prevention of coccidiosis in commercial poultry production.

Known methods of obtaining tarmacced the chlorination of 2,6-dimethyl-4(1H)pyridone gaseous chlorine [1] or potassium chlorate in the environment of hydrochloric acid [2] the Disadvantages of these methods are the dangers of using chlorine gas, a deficit of potassium chlorate and expensive technological equipment made of titanium, enameled cast iron.

Known bezopasny output of tarmacced to 85% However, a significant drawback of this method is the necessity of neutralization of up to 30 litres of waste water per 1 kg of the finished product without regard to the wash water, what complicates the technology and increases the cost of tarmacced.

The aim of the invention is to increase the output of tarmacced and reduce waste production.

This goal is achieved by electrochemical chlorination of 2,6-dimethyl-4(1H)pyridone in an aqueous solution at econometricians the anodes (ORT) in membrane electrolysis at a current density of from 0.84 to 2.0 kA/m2, volumetric current density 15-20 A/l, a temperature of 15-25oWith NaCl concentration of 200-300 g/l at pH 2-9, the concentration of 2,6-dimethyl-4(1H)pyridone 5-20 g/l and at a dose in the anode electrolyte saturated aqueous solution of 2,6-dimethyl-4(1H)pyridone. The method allows to obtain tarmacced with access to 87.9% and a small amount of waste (5 l/kg of product, taking into account the wash water). The advantage of this method is the ability to obtain a scarce sodium hydroxide, which is formed in the cathode space of the electrolyzer (2 mol per mol of tarmacced with metering to neutralize accumulated in the anolyte hydrochloric acid).

The scheme of the laboratory setup is given on the drawing, where: 1 cell, 2 - capacity anolyte, 3 capacity Catolica, 4 pumps, 5 knock-out box.

Methodology elektrolizerami 2,6-dimethyl-4(1H)pyridone output tarmacced presented in table.1. Results ten of electrolysis in the series are presented in table.2.

Example 1. In the device 2, provided with a stirrer and a thermometer (see diagram), is filled with 800 ml of an aqueous solution containing 5 g of 2,6-dimethyl-4(1H)pyridone and 200 g NaCl anolyte. In the apparatus 3 is filled with 600 ml of 2% aqueous solution of NaOH catholyte. Included pumps 4 and terminal membrane filtermessage cell 1 is energized, the corresponding amperage 15 A. (Square of ORTA 120 cm2the current density of 1.25 kA/m2, volumetric current density of 18.7 A/l) cold water over the shirt apparatus 2, the temperature of the anolyte is maintained in the range of 15-25oC. during the electrolysis in the apparatus 2 is dosed with 100 ml saturated aqueous solution of 2,6-dimethyl-4(1H)pyridone containing 10 g of the basic substance with a speed that ensures the constancy of its concentration in the anolyte and 10% aqueous NaOH solution to maintain the pH of the anolyte within 2-9 (pH of the solution is controlled by pH-meter).

By passing 4 F electricity per mole of 2,6-dimethyl-4(1H)pyridone, dozirovannogo in the form of saturated solution (after 32 minutes after switching on the unit), voltage is removed and the contents of the apparatus 2, which is an aqueous suspension of tarmacced, filtered to orangedental-4(1H)pyridone. Tarmacced on the funnel is washed, and then dried in a drying Cabinet at a temperature of 60-70oC to constant weight.

The output of tarmacced 14,44 g (92,6%).

Found: C 43,9; H 3,4; 7,4; Cl 37,2% C7H7NOCl2< / BR>
Calculated: C 43,7; H 3,6; 7,3; Cl 37,0%

The amount spent anolyte 780-800 Jr. due to electroosmotic migration of water in the catholyte volume of the anolyte during electrolysis is reduced to 700-720 mm. to compensate For the volume of anolyte to the original during electrolysis is added to 80-100 ml of water in a saturated dosing of a solution of 2,6-dimethyl-4(1H)pyridone. In the anolyte is added 20 g of NaCl, and then carried out the following electrolysis. In the subsequent electrolysis of 2,6-dimethyl-4(1H)pyridone is added to the anolyte only in the form of saturated solution for dosing.

Total removal of the product from the series (see tab.2) is 142,4 g (91.2 per cent), the total volume of wastewater, including washing, 800 g Specific volume of wastewater is 5.6 l/kg for the series, which is considerably lower than in known methods of obtaining tarmacced.

Specific volume of wastewater can be reduced by increasing the number of syntheses on a single electrolyte.

Example 2. The method and conditions of the experiment, Asia hydrochloric acid is used 15% aqueous solution of Na2CO3.

The output of tarmacced 14,18 g (90,8%).

Carrying out electrolysis at a temperature below 15oWith no increases yield, but requires additional energy consumption for cooling, the temperature increases above 25oWith reduces the yield of the target product.

In the electrolysis, where the current density is not more than 1 kA/m2used cation-exchange membrane MK-40, in other fluoropolymer membrane MF-SC. Tests at higher current density was not conducted, since 2 kA/m2the limiting current density for a more sustainable membrane MF-SC.

The choice of the analyte is determined corrosion resistance ORT, equipment and quality of the product. ORT allows long periods of operation at pH 1,65, in addition, at pH<2 in chloride solutions begins intensive corrosion of stainless steels. Therefore, the experiments at pH<2 were not conducted. At pH>9 the finished product is brown in color and does not meet SPECIFICATIONS. The experiments showed no dependence of the yield of tarmacced from the pH of the anolyte in this range.

The choice of anode material ORT is determined by its adaptability, low U [4] according to which higher outputs chlorinated in electrochemical chlorination observed when using anodes made of this material.

Thus, conducting electrolysis under optimal conditions allows to obtain tarmacced with access 87,9-of 92.6% with a minimum amount of liquid waste 5 l/kg of product, plus NaOH 0.6 to 0.8 kg/kg of synthesized tarmacced.

The organization of production, this method can form the basis of modern high-performance low-waste technology of obtaining tarmacced.

The way to obtain 2,6-dimethyl-3,5-dichloro-4(IN)of the pyridone by chlorination of 2,6-dimethyl-4(IH)pyridone in an aqueous medium, characterized in that carry out the electrolysis in membrane electrolyzer on ksirodarnavasambhavam the anode when the anode current density is 0.84 a 2.0 kA/m2, volumetric current density of 15 to 20 A/l, a temperature of 15 25oWith and while maintaining a pH of 9, the concentration of 2,6-dimethyl-4(IH) pyridone 5 20 g/l and the concentration of sodium chloride 200 to 300 g/l by dosing into the anode electrolyte reagents and aqueous hydroxide solution or sodium carbonate.

 

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