The line for imidazole

 

(57) Abstract:

Usage: the synthesis of heterocyclic compounds. The inventive line receiving antifungals, including installed downstream and related vehicles module preparation of ammonium-formalin solution and module synthesis of imidazole with installation distillation of the ammonia-alkaline of distillate from the reaction mixture, installed for the module synthesis of imidazole, and the module vacuum distillation, placed at the end of the line, and the module synthesis of imidazole piped to install the distillation of the ammonia-alkaline distillate, and means of transportation VAT residue module vacuum distillation. The technical result - improving the quality of the target product and increase output. 1 Il.

The invention relates to the field of organic chemistry, in particular to methods of synthesis of heterocyclic compounds and can be used in the production of imidazole needed to obtain drugs and sorbents.

Known apparatus-technological line for imidazole, in which the course of the process established with the ü synthesis of imidazole (1).

In the famous line getting imidazole is in the process of interaction of glyoxal with aqueous solutions of ammonia and formaldehyde at a temperature of 65 - 70oC and subsequent exposure of the reaction mixture for 1 hour for intermolecular condensation of glyoxal, ammonia and formaldehyde in aqueous solution according to the scheme:

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Famous line obtain imidazole is closest to the proposed and selected as a prototype.

The disadvantages of the known line is the low output and high pollution received technical imidazole impurities.

This is due to the fact that due to the complex nature of the reaction of condensation and high reactivity of the starting substances along with imidazole, the formation of by-products, in particular 2,2-bis-imidazole, urotropine, 4(5)-oximetronidazole, derivatives of formic acid, etc.

The objective of the invention is to improve the quality and yield of imidazole.

This object is achieved in that the line for antifungals that include the installed downstream and related vehicles module preparation of ammonium-parselocale distillate from the reaction mixture, installed for the module synthesis of imidazole, and the module vacuum distillation, placed at the end of the line, and the module synthesis of imidazole piped to install the distillation of the ammonia-alkaline distillate, and means of transportation VAT residue module vacuum distillation.

The advantage of the proposed line is that due to the evaporation of the solvent by distillation under technical vacuum ammonium-alkaline distillate, allows vacuum distillation VAT residue, representing a technical imidazole, with the release fractions containing the imidazole with a mass fraction of the main substance of ~96% with a yield of 60% of theoretical, calculated on the formaldehyde.

The invention is illustrated in the drawing, which schematically illustrates the line, General view.

The line for imidazole according to the scheme: intermolecular condensation of glyoxal, ammonia and formaldehyde in water), evaporation of the solvent from the condensate by distillation of the ammonia-alkaline distillate and vacuum distillation VAT residue emitting fraction of imidazole with mass fractions of the basic substance is 96%, contains installed along the technology is a new solution, module 2 synthesis of imidazole, installation 3 distillation of the ammonia-alkaline distillate and module 4 vacuum distillation.

Module 1 preparation of ammonium-formalin solution is designed to prepare the mixture of ammonia and formalin and includes the reactor 5 with a cooled jacket 6, the supply 7 and the drain 8 of the nozzle and the mixer 9, the measuring device 10 of the ammonia and the measuring device 11 formalin, United means of transportation of product from the supply pipe 7 of the reactor 5.

Module 1 means of transportation ammonium-formalin mixture connected with the reactor 12 synthesis of imidazole module 2.

Module 2 synthesis of imidazole is a reactor 12 with a heated jacket 13, a mixer 14, the supply 15 and the drain 16 of the nozzle and the measuring device 17 glyoxal, United pipeline.

Module 2 is connected by a steam line installation 3 distillation of the ammonia-alkaline distillate, and means of transportation VAT residue module 4 vacuum distillation.

Installation 3 distillation of the ammonia-alkaline distillate performed, for example, in the form of three heat exchangers 18', 18", 18"' with connections to input 19 output 20 of the distillate and the collector 21 of distilled water, sequentially interconnected troop emitting and collecting three fractions of distillate and made in the form of electrically heated reactor 22 with the Packed column 23, two heat exchangers 24', 24", connected in series with the column 23 of the reactor 22, and collections 25, 26, 27 of the first, second and third fractions of the distillate, respectively, each of which is piped to the heat exchanger 24, and vacuumbroom sequentially connected through the vacuum receiver 28 to a vacuum pump 29.

Transport pipelines line equipped with shut-off devices and the actuator (not shown).

The line work is carried out as follows.

In a sealed reactor 5 module 1 through the pipe 7 from the measuring device 10 load 25% ammonia solution and the flow of brine in the jacket 6 of the reactor is cooled with stirring by a stirrer 9 to a temperature of 0oC.

Then from the measuring device 11 in the reactor 5 with continuous stirring load 37% technical solution of formalin. Ammonium-formalin mixture is cooled to a temperature of 0 to 5oC and then compressed nitrogen gas discharged from the reactor 5 through the drain pipe 9 in a sealed reactor 12 module 2.

In the reactor 12 under stirring ammonia-formalin mixture through pipe 15 download from the measuring device 17 40% solution of glyoxal. When loading glyoxal reaction mixture in reactor heated under stirring up to a temperature of 70oC and kept at this temperature for 1 hour.

After exposure to the reactor 12 is connected under technical vacuum heat exchangers 18' - 18"' and a collection of 21 installation 3.

Under vacuum with stirring and the temperature in pairs ~60oC from the reactor 12 successively through the heat exchangers 18' and 18"', the cooled circulating water, and the heat exchanger 18"' cooled brine is evaporated in a collection of 21 installation 3 ammonium-alkaline distillate until the termination of the flow of the distillate.

Ammonium-alkaline distillate from collector 21 through the bottom of the descent by gravity drained into the sewer of histochem.

VAT residue, representing a technical imidazole, from the reactor 12 with compressed nitrogen discharged through the drain pipe 16 into the reactor 22 module 4 for vacuum distillation.

In the process of distillation from the reactor 22 when the vacuum Pleave= 5.333 kPa through the heat exchangers 24' and 24", the cooled circulating water, successively distilled off at a temperature in pairs:

120 - 144oC - the first fraction of distillate,

144 - 163oC - the second fraction and

163 - 169oC - the third faction, representing the imidazole with a mass fraction of the main substance of 96%.

The first coat is">

The second fraction is sent to the collector 26 and then fed to the repeated vacuum distillation to extract the contained imidazole.

The fraction of imidazole take in a heated collector 27.

When the temperature drops in pairs less than 160oC and at a pressure Pleave= 5.333 kPa flow shoulder straps stop and distillation finish. At the end of the distillation reactor 22 and collections 25, 26 and 27 is disconnected from the vacuum pump 29.

VAT residue in the reactor 22 is cooled to a temperature of 100oC and unloaded by gravity through the bottom of the descent in a special container and then burn.

In the distillation, taking into account product extracted from the second fraction, the output of imidazole is 59.75% of theoretical, calculated on the formaldehyde content of the basic substance in the finished product 96%.

Thus, the proposed line by distinctive signs, made according to the invention, allows to increase the output and quality of the product.

The line for antifungals that include the dipstick formalin, dipstick solution of glyoxal, a reactor for the preparation of ammonium formalinova solution and synthesis of imidazole, the installation for the distillation of ku is midazole posted separately belted respectively cooling and heating shirts and are connected by a pipeline for the transportation of ammonia and formalin solution, the line is supplied is connected to the reactor for the preparation of ammonium-formalin solution in the measuring device of an aqueous solution of ammonia and steam line connected to the reactor for the synthesis of imidazole install the distillation of the ammonia-alkaline distillate, the apparatus for distillation VAT residue connected to the reactor for the synthesis of imidazole drain pipe and includes a vacuum pump, dipstick formalin connected to the reactor for the preparation of ammonium-formalin solution, and dipstick solution of glyoxal is connected to the reactor for the synthesis of imidazole.

 

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CFN< / BR>
where R represents a hydrogen atom or methyl;

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13 cl, 18 ex, 1 tbl

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3 ex

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17 cl, 2 tbl, 74 ex

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