Line obtain bis (1-vinylimidazole) zincdiacetate

 

(57) Abstract:

The line is designed to obtain complexes of substituted heterocyclic azole series, in particular for the synthesis of bis(1-vinylimidazole)zincdiacetate. Line obtain bis(1-vinylimidazole)zincdiacetate includes installed downstream and related vehicles module synthesis of the complex bis(1-vinylimidazole)zincdiacetate and module selection of the target product, the module dissolution of 1-vinylimidazole, located at the beginning of the line, and the module dehydration of zinc diacetate, placed before the module synthesis of the complex, this module dissolution of 1-vinylimidazole and module dehydration of zinc diacetate connected vehicles with module synthesis of the complex, and the last module selection of the target product. Increases the yield of the target product and reduces the cost allocation of the complex from the mother liquor. 1 C.p. f-crystals, 1 Il.

The invention relates to the field of organic chemistry, in particular, to techniques for the production of complexes of substituted heterocyclic compounds isologo range and can be used for the synthesis of bis(1-vinylimidazole)zincdiacetate (alzola the l)zincdiacetate, representing the complex compound in which two molecules of 1-vinylimidazole associated with one molecule of zinc diacetate (RF patent N 2038079, class A 61 K 31/15, 1995).

Also known as safener carbon monoxide bis(1-vinylimidazole)zincchloride obtained in a process line in which the course of the process set connected vehicles reactor for the synthesis of the target product with attached measuring tanks organic solvent, 1-vinylimidazole and anhydrous zinc salts, the apparatus for separation of solid and liquid phases with a connected her collection of stock solution and vacuum-drying for dehydration of the solid phase (ed. mon. USSR N 1822155, class C 07 F 3/06, 1991). The famous line is closest to the proposed and selected as a prototype. The disadvantages of the known line is the low efficiency of obtaining bis(1-vinylimidazole)zincdiacetate because of the high cost of removing a target product and its low output.

This is due to the fact that famous line synthesis of bis(1-vinylimidazole)zincdiacetate is accompanied by dissolution of the resulting complex in the mother solution, due to the high content crystallizations)zincdiacetate in the mother solution, and thus contributes to increased yield and reduced production costs. This is achieved by the fact that the line receiving bis(1-vinylimidazole)zincdiacetate, including its synthesis reactor, mernik, acetone-ether mixture, 1-vinylimidazole and anhydrous zinc diacetate and installation for the separation of solid and liquid phases with a connected her collection of mother liquor, according to the invention is equipped with a reactor for the preparation of a solution of 1-vinylimidazole in acetone-ether mixture, the dipstick dihydrate zinc acetate and installation of its dehydration, placed at the beginning of the line and dipstick solution of 1-vinylimidazole in acetone-ether mixture, connected to the output of the reactor, its preparation and the inlet of the reactor for the synthesis of bis(1-vinylimidazole)zincdiacetate, and gages 1-vinylimidazole, acetone-air mixture is connected to the input of the reactor preparation of a solution of 1-vinylimidazole in acetone-ether mixture, dipstick dihydrate zinc acetate is connected with the input set him hydrated and dipstick anhydrous zinc diacetate - last exit and entrance of the reactor for the synthesis of bis(1-vinylimidazole)zincdiacetate, the output of which is connected to an apparatus for separation of solid and liquid phases. The installation of the dehydration of the dihydrate zinc acetate is a vacuum dryer, and the unit for time is odara to ensure the possibility of pre-dissolution 1-vinylimidazole in acetone-ether mixture and dehydration zinc diacetate, is achieved by preventing the dissolution of the complex bis(1-vinylimidazole)zincdiacetate in the mother solution in the process of its synthesis. The result is a complete bicrystalline complex from the mother liquor and their separation by density under the influence of centrifugal forces that increase output and reduce costs.

Line obtain bis(1-vinylimidazole)zincdiacetate scheme: the dissolution of 1-vinylimidazole in acetone-ether mixture, the preparation of a suspension of anhydrous zinc diacetate in acetone-ether mixture, the interaction of 1-vinylimidazole with the diacetate of zinc in the environment of acetone and ether with the formation of complex compounds

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and its subsequent separation from the mother liquor contains interconnected downstream vehicles module 1 dissolved 1-vinylimidazole in acetone-ether mixture, module 2 dehydration of zinc diacetate, module 3 synthesis of bis(1-vinylimidazole)zincdiacetate and module 4 selection of the target product from the mother liquor (see drawing).

The invention consists in that, due prior to the dissolution of 1-vinylimidazole in acetone-ether mixture and dehydration zinc diacetate is in the mother solution. In turn, prevent the dissolution of the complex in the mother solution, allows it to complete the crystallization, which increases product yield and reducing the cost allocation of the complex from the mother liquor.

Module 1 is designed for preparation of a solution of 1-vinylimidazole in acetone-ether mixture and represents the reactor 5 with jacket 6, the supply 7 and the drain 8 of the nozzle and the mixer 9 and the tanks 10, 11 acetone-ether mixture and 1-vinylimidazole, itself connected by a pipe with the supply pipe 7 of the reactor 5.

Module 2 is designed to produce anhydrous zinc diacetate and represents a vacuum dryer with 12 heated by a jacket 13, the boot 14 and discharge 15 manholes and Gribkova shaft 16 and pump 17 dihydrate zinc acetate, connected by pipeline with the dryer 12.

Module 1 and module 2 means of transportation of the product are connected respectively with the measuring device 24 solution of 1-vinylimidazole and measuring device 23 of anhydrous zinc diacetate module 3.

Module 3 is designed for preparation of a suspension of anhydrous zinc acetate in a mixture of acetone and ether and synthesis of complex 1-vinylimidazole with zinc diacetate in acetone-terrestrial environment and performance, the om with the supply pipe reactor gages 23, 24 anhydrous zinc diacetate and a solution of 1-vinylimidazole in acetone-ether mixture, respectively.

Module 3 is connected by a pipeline with the centrifuge 25 module 4.

Module 4 is designed to separate the complex bis(1-vinylimidazole)zincdiacetate from the mother liquor and is an installation of 25 to separate the solid and liquid phases, made for example in the form of a centrifuge and a collection of 26 the mother liquor, United pipeline.

The hotline is as follows.

In a clean, dry and airtight reactor 5 module 1 is poured from the measuring device 10 acetone-ether mixture (1: 1) and from the measuring device 11 download with stirring, 1-vinylimidazole, the mass in the reactor is stirred for 10 min and then compressed nitrogen into the reactor (not shown) is discharged through the drain pipe 8 to the measuring device 24 module 3.

From the measuring device 17 in the vacuum dryer 12 module 2 load dihydrate zinc acetate and stirring Gribkova shaft 16 at a temperature of 80-100oC and a pressure of 80 kPa dehydrate until the zinc content in the zinc diacetate 35-36%. After drying the anhydrous zinc diacetate unloaded from the dryer 12 and transported to the measuring device 23 module 3.

In a clean, dry and airtight reactor 18 Inca.

The start of hot water in the jacket 19 of the reactor suspension of zinc diacetate in acetone-ether medium is heated to a temperature of 25oC. After that, the reactor from the measuring device 24 is slowly poured with continuous stirring a solution of 1-vinylimidazole in acetone-ether mixture.

At the end of the loading solution of 1-vinylimidazole mass in the reactor is stirred for 1 h Then the flow of brine in the jacket of the reactor, the reaction mass is then cooled with stirring to a temperature of 5oC and kept at this temperature until complete crystallization of bis(1-vinylimidazole)zincdiacetate. After crystallization of the complex mass is unloaded from the reactor through the drain pipe and serves on the separation of the solid phase from the mother liquor in a centrifuge 25 module 4.

In the centrifuge 25 complex bis(1-vinylimidazole)cindicates separated by density from the mother liquor. The mother liquor is taken in the compilation of 26 and serves on the regeneration of acetone, and highlighted the complex unloaded from cetrifuge 25 and serves for filling (not shown).

Thus, the proposed line, allowing synthesis of the complex bis(1-vinylimidazole)zincdiacetate in conditions conducive to the crystallization of the comp is hodom to 89-93% of theoretical, counting 1-vinylimidazole, when the content of pharmacopoeial product 99%. Thus providing the possibility of separation of the complex and the mother liquor density reduces the cost allocation of the finished product.

The sources of information.

1. Patent N 2038079, 6A 61 K 31/315, 1995. The decision to grant a patent on the application N 2233525/04 (003307) from 1.03.78, C 07 S 1/00.

1. Line obtain bis(1-vinylimidazole)zincdiacetate includes a reactor for the synthesis of bis(1-vinylimidazole)zincdiacetate, mernik, acetone-ether mixture, 1-vinylimidazole and anhydrous zinc diacetate, vacuum dryer with loading and unloading hatches, installation for the separation of solid and liquid phases with a connected her collection of mother liquor, characterized in that it is equipped with a sealed reactor for preparation of a solution of 1-vinylimidazole in acetone-air mixture, is connected to both reactors supply pipe and drain pipe connected to the boot hatch vacuum-drying the dipstick dihydrate zinc acetate, connected to the drain pipe reactor for preparation of a solution of 1-vinylimidazole in acetone-air mixture and to the supply outlet of the reactor for the synthesis of bis(1-vinylimidazole)zincdiacetate the dipstick solution is sealed, standard 1-vinylimidazole in acetone-air mixture is connected to the supply pipe reactor for preparation of a solution of 1-vinylimidazole in acetone-ether mixture, dipstick anhydrous zinc diacetate is connected to the discharge manhole vacuum dryer and to the supply outlet of the reactor for the synthesis of bis(1-vinylimidazole)zincdiacetate, the apparatus for separation of solid and liquid phases is connected to the drain pipe reactor for the synthesis of bis(1-vinylimidazole)zincdiacetate.

2. Line p. 1, characterized in that the device for separation of solid and liquid phases is made in the form of a centrifuge.

 

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