CN218262334U - Production system for dimethylamino thioacetyl as raw material of nizatidine skeleton - Google Patents
Production system for dimethylamino thioacetyl as raw material of nizatidine skeleton Download PDFInfo
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- CN218262334U CN218262334U CN202222335983.7U CN202222335983U CN218262334U CN 218262334 U CN218262334 U CN 218262334U CN 202222335983 U CN202222335983 U CN 202222335983U CN 218262334 U CN218262334 U CN 218262334U
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Abstract
The utility model discloses a production system of a nizatidine skeleton raw material dimethylamino thioacetyl, which comprises a hydroxyl acetonitrile metering storage tank arranged at the front end; the rear end of the hydroxyl acetonitrile metering storage tank is connected with a dimethylamino acetonitrile reaction kettle and a crystallization kettle in parallel through a pipeline; the upper part of the dimethylamino acetonitrile reaction kettle is connected with a dimethylamine head tank through a pipeline; the rear end of the dimethylamino acetonitrile reaction kettle is connected with a dimethylamino thioacetamide synthesis kettle through a pipeline; a toluene metering storage tank and a liquid caustic soda elevated tank are connected to the dimethylamino thioacetamide synthesis kettle through pipelines; the rear end of the dimethylamino thioacetamide synthesis kettle is connected to the crystallization kettle through a pipeline; the crystallization kettle is connected with a sodium cyanide head tank through a pipeline; the rear end of the crystallization kettle is connected with a centrifugal machine through a pipeline; the rear end of the centrifugal machine is connected with a toluene mother liquor underground storage tank through a pipeline; the equipment can achieve more reasonable arrangement of a production system and high production efficiency.
Description
Technical Field
The utility model belongs to bulk drug processing equipment field, concretely relates to nizatidine skeleton raw materials dimethylamino thioacetyl production system.
Background
Nizatidine is a potent H2 receptor antagonist, acts on gastric acid-secreting cells, blocks gastric acid formation and lowers basal gastric acid, and also inhibits gastric acid secretion caused by food and chemical stimuli. Is suitable for active duodenal ulcer and gastric ulcer, and can be used for preventing duodenal ulcer after healing.
The existing production process of nizatidine is still not perfect, and many process parameters need to be further confirmed and optimized. Particularly, the key framework raw material dimethylamino thioacetyl of the product is synthesized at the present stage, the synthesis route of the product is old, and the product yield is low. The process operation difficulty is high, and the prior equipment cannot achieve ideal yield; by optimizing and adjusting the process of the special equipment and facilities, the production process of the skeleton raw material dimethylamino thioacetyl is realized to achieve the purposes of reducing the production cost and improving the production efficiency.
SUMMERY OF THE UTILITY MODEL
The utility model provides a nizatidine skeleton raw materials dimethylamino thioacetyl production system, the use of this equipment can reach that production system arranges more rationally, the efficiency that production efficiency is high.
In order to achieve the above object, the utility model provides a following technical scheme: a production system for nizatidine skeleton raw material dimethylamino thioacetyl comprises a hydroxy acetonitrile metering storage tank arranged at the front end; the rear end of the hydroxyl acetonitrile metering storage tank is connected with a dimethylamino acetonitrile reaction kettle and a crystallization kettle in parallel through pipelines; the upper part of the dimethylamino acetonitrile reaction kettle is connected with a dimethylamine head tank through a pipeline; the rear end of the dimethylamino acetonitrile reaction kettle is connected with a dimethylamino thioacetamide synthesis kettle through a pipeline; the dimethylamino thioacetamide synthesis kettle is connected with a toluene metering storage tank and a liquid caustic soda head tank through pipelines; the rear end of the dimethylamino thioacetamide synthesis kettle is connected to the crystallization kettle through a pipeline; the crystallization kettle is connected with a sodium cyanide head tank through a pipeline; the rear end of the crystallization kettle is connected with a centrifugal machine through a pipeline; the rear end of the centrifugal machine is connected with a toluene mother liquor underground storage tank through a pipeline; the rear end of the underground toluene mother liquor storage tank is connected with a toluene distillation kettle through a pipeline; the rear end of the toluene distillation kettle is connected with a high-low boiling storage tank through a pipeline.
Preferably, the front end of the dimethylamine head tank is connected with a dimethylamine metering storage tank through a pipeline.
Preferably, the dimethylamino acetonitrile reaction kettle is connected with a low boiling tank and a dimethylamino acetonitrile storage tank in parallel through pipelines.
Preferably, the front end of the sodium cyanide head tank is connected with a sodium cyanide aqueous solution tank through a pipeline.
Preferably, the dimethylamino thioacetamide synthesis kettle is connected with a first condenser through a pipeline.
Preferably, the crystallization kettle is connected with a second condenser through a pipeline.
Preferably, the toluene distillation still is connected with a third condenser through a pipeline.
Preferably, a fourth condenser is arranged on a pipeline between the dimethylamino acetonitrile reaction kettle and the low-boiling tank.
Compared with the prior art, the beneficial effects of the utility model are that: the new production system enables the production process of the dimethylamino thioacetyl to reduce the production cost, improve the production efficiency and ensure that the arrangement of the production system is more reasonable.
Other features of the present disclosure and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.
Drawings
In order to more clearly illustrate the embodiments of the present disclosure or technical solutions in related arts, the drawings used in the description of the embodiments or related arts will be briefly introduced below, it is obvious that the drawings in the following description are only embodiments of the present disclosure, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an overall view of the production system of the present invention;
in the figure: 1. the device comprises a hydroxyl acetonitrile metering storage tank, 2, a dimethylamino acetonitrile reaction kettle, 3, a dimethylamine head tank, 4, a dimethylamino thioacetamide synthesis kettle, 5, a toluene metering storage tank, 6, a liquid caustic soda head tank, 7, a crystallization kettle, 8, a sodium cyanide head tank, 9, a centrifuge, 10, a toluene mother liquor underground storage tank, 11, a toluene distillation kettle, 12, a high-low boiling storage tank, 13, a dimethylamine metering storage tank, 14, a low-boiling tank, 15, a dimethylamino acetonitrile storage tank, 16, a sodium cyanide water solution tank, 17, a first condenser, 18, a second condenser, 19, a third condenser, 20 and a fourth condenser.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Unless specifically stated otherwise, the relative arrangement of parts and steps, numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the present invention. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
For ease of description, spatially relative terms such as "over 8230," "upper surface," "above," and the like may be used herein to describe the spatial positional relationship of one device or feature to other devices or features as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary terms "at 8230; \8230; above" may include both orientations "at 8230; \8230; above" and "at 8230; \8230; below". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Referring to fig. 1, the present invention provides a technical solution: a production system of nizatidine skeleton raw material dimethylamino thioacetyl comprises a hydroxy acetonitrile metering storage tank 1 arranged at the front end; the rear end of the glycolonitrile metering storage tank 1 is connected with a dimethylamino acetonitrile reaction kettle 2 and a crystallization kettle 7 in parallel through pipelines; the upper part of the dimethylamino acetonitrile reaction kettle 2 is connected with a dimethylamine head tank 3 through a pipeline; the rear end of the dimethylamino acetonitrile reaction kettle 2 is connected with a dimethylamino thioacetamide synthesis kettle 4 through a pipeline; a toluene metering storage tank 5 and a liquid caustic soda elevated tank 6 are connected on the dimethylamino thioacetamide synthesis kettle 4 through pipelines; the rear end of the dimethylamino thioacetamide synthesis kettle 4 is connected to the crystallization kettle 7 through a pipeline; the crystallization kettle 7 is connected with a sodium cyanide head tank 8 through a pipeline; the rear end of the crystallization kettle 7 is connected with a centrifuge 9 through a pipeline; the rear end of the centrifugal machine 9 is connected with a toluene mother liquor underground storage tank 10 through a pipeline; the rear end of the toluene mother liquor underground storage tank 10 is connected with a toluene distillation kettle 11 through a pipeline; the rear end of the toluene distillation kettle 11 is connected with a high-low boiling storage tank 12 through a pipeline.
The front end of the dimethylamine head tank 3 is connected with a dimethylamine metering storage tank 13 through a pipeline. The dimethylamino acetonitrile reaction kettle 2 is connected with a low boiling tank 14 and a dimethylamino acetonitrile storage tank 15 in parallel through pipelines. The front end of the sodium cyanide head tank 8 is connected with a sodium cyanide water solution tank 16 through a pipeline. The dimethylamino thioacetamide synthesis kettle 4 is connected with a first condenser 17 through a pipeline. The crystallization kettle 7 is connected with a second condenser 18 through a pipeline. The toluene distillation still 11 is connected to a third condenser 19 through a pipe. A fourth condenser 20 is arranged on a pipeline between the dimethylamino acetonitrile reaction kettle 2 and the low-boiling tank 14.
During production, a quantitative amount of hydroxyacetonitrile (the content of the hydroxyacetonitrile is 40%) is added into a dimethylaminoacetonitrile reaction kettle 2 through a hydroxyacetonitrile metering tank 1, the mixture is stirred for 30 minutes at normal temperature, a dimethylamine overhead tank 3 dropwise adding valve is opened after stirring is finished, dimethylamine (the content of the dimethylamine is 40%) is dropwise added at normal temperature, the temperature is kept for 2 hours at about 25 ℃ after the dropwise adding is finished, and the feed liquid is prepared to be pumped into a dimethylaminothioacetamide synthesis kettle 4 after the temperature is kept.
Passing through a 2000L toluene metering tank 5, adding quantitative toluene into a dimethylamino thioacetamide synthesis kettle 4, opening a jacket freezing inlet-outlet valve of the dimethylamino thioacetamide reaction kettle 4, cooling the toluene solution to 10-20 ℃, pumping the dimethylamino acetonitrile solution into the dimethylamino thioacetamide reaction kettle 4 after the toluene solution is cooled, stirring and controlling the temperature to 10-20 ℃, adding phosphorus pentasulfide in batches at the temperature, opening a jacket steam inlet-outlet valve of the dimethylamino thioacetamide reaction kettle 4 after the materials are added, heating to 70-80 ℃ (the steam pressure is less than or equal to 0.15 Mpa), reacting for 8 hours at the temperature, closing the jacket steam inlet-outlet valve of the dimethylamino thioacetamide reaction kettle 4, standing and layering for 12 hours, removing a water layer through a long sight cup of the dimethylamino thioacetamide reaction kettle 4, and pumping a toluene layer into a crystallization kettle 7. Opening a freezing inlet and outlet valve of a jacket of the crystallization kettle 7, cooling the feed liquid to below 30 ℃, performing solid-liquid separation by a centrifuge 9, filling a wet product of the dimethylamino thioacetamide into a special barrel, and drying. Toluene is put into a toluene mother liquor underground storage tank 10 and then is put into a toluene distillation kettle 11 for distillation.
Example 1:
a production system of nizatidine skeleton raw material dimethylamino thioacetyl comprises a hydroxy acetonitrile metering storage tank 1 arranged at the front end; the rear end of the glycolonitrile metering storage tank 1 is connected with a dimethylamino acetonitrile reaction kettle 2 and a crystallization kettle 7 in parallel through pipelines; the upper part of the dimethylamino acetonitrile reaction kettle 2 is connected with a dimethylamine head tank 3 through a pipeline; the rear end of the dimethylamino acetonitrile reaction kettle 2 is connected with a dimethylamino thioacetamide synthesis kettle 4 through a pipeline; the dimethylamino thioacetamide synthesis kettle 4 is connected with a toluene metering storage tank 5 and a liquid caustic soda elevated tank 6 through pipelines; the rear end of the dimethylamino thioacetamide synthesis kettle 4 is connected to the crystallization kettle 7 through a pipeline; the crystallization kettle 7 is connected with a sodium cyanide head tank 8 through a pipeline; the rear end of the crystallization kettle 7 is connected with a centrifuge 9 through a pipeline; the rear end of the centrifugal machine 9 is connected with a toluene mother liquor underground storage tank 10 through a pipeline; the rear end of the toluene mother liquor underground storage tank 10 is connected with a toluene distillation kettle 11 through a pipeline; the rear end of the toluene distillation kettle 11 is connected with a high-low boiling storage tank 12 through a pipeline.
Example 2:
a production system of nizatidine skeleton raw material dimethylamino thioacetyl comprises a hydroxyacetonitrile measuring storage tank 1 arranged at the front end; the rear end of the glycolonitrile metering storage tank 1 is connected with a dimethylamino acetonitrile reaction kettle 2 and a crystallization kettle 7 in parallel through pipelines; the upper part of the dimethylamino acetonitrile reaction kettle 2 is connected with a dimethylamine head tank 3 through a pipeline; the rear end of the dimethylamino acetonitrile reaction kettle 2 is connected with a dimethylamino thioacetamide synthesis kettle 4 through a pipeline; a toluene metering storage tank 5 and a liquid caustic soda elevated tank 6 are connected on the dimethylamino thioacetamide synthesis kettle 4 through pipelines; the rear end of the dimethylamino thioacetamide synthesis kettle 4 is connected to the crystallization kettle 7 through a pipeline; the crystallization kettle 7 is connected with a sodium cyanide head tank 8 through a pipeline; the rear end of the crystallization kettle 7 is connected with a centrifuge 9 through a pipeline; the rear end of the centrifugal machine 9 is connected with a toluene mother liquor underground storage tank 10 through a pipeline; the rear end of the toluene mother liquor underground storage tank 10 is connected with a toluene distillation kettle 11 through a pipeline; the rear end of the toluene distillation kettle 11 is connected with a high-low boiling storage tank 12 through a pipeline. The front end of the dimethylamine head tank 3 is connected with a dimethylamine metering storage tank 13 through a pipeline. The dimethylamino acetonitrile reaction kettle 2 is connected with a low boiling tank 14 and a dimethylamino acetonitrile storage tank 15 in parallel through pipelines. The front end of the sodium cyanide head tank 8 is connected with a sodium cyanide water solution tank 16 through a pipeline. The dimethylamino thioacetamide synthesis kettle 4 is connected with a first condenser 17 through a pipeline. The crystallization kettle 7 is connected with a second condenser 18 through a pipeline. The toluene distillation still 11 is connected with a third condenser 19 through a pipeline. A fourth condenser 20 is arranged on a pipeline between the dimethylamino acetonitrile reaction kettle 2 and the low-boiling tank 14.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A production system of nizatidine skeleton raw material dimethylamino thioacetyl is characterized in that: the production system comprises a hydroxyacetonitrile metering storage tank (1) arranged at the front end; the rear end of the glycolonitrile metering storage tank (1) is connected with a dimethylamino acetonitrile reaction kettle (2) and a crystallization kettle (7) in parallel through pipelines; the upper part of the dimethylamino acetonitrile reaction kettle (2) is connected with a dimethylamine head tank (3) through a pipeline; the rear end of the dimethylamino acetonitrile reaction kettle (2) is connected with a dimethylamino thioacetamide synthesis kettle (4) through a pipeline; the dimethylamino thioacetamide synthesis kettle (4) is connected with a toluene metering storage tank (5) and a liquid caustic soda elevated tank (6) through pipelines; the rear end of the dimethylamino thioacetamide synthesis kettle (4) is connected to the crystallization kettle (7) through a pipeline; the crystallization kettle (7) is connected with a sodium cyanide head tank (8) through a pipeline; the rear end of the crystallization kettle (7) is connected with a centrifugal machine (9) through a pipeline; the rear end of the centrifugal machine (9) is connected with a toluene mother liquor underground storage tank (10) through a pipeline; the rear end of the toluene mother liquor underground storage tank (10) is connected with a toluene distillation kettle (11) through a pipeline; the rear end of the toluene distillation kettle (11) is connected with a high-low boiling storage tank (12) through a pipeline.
2. The system for producing raw material dimethylamino thioacetyl as nizatidine skeleton according to claim 1, characterized in that: the front end of the dimethylamine head tank (3) is connected with a dimethylamine metering storage tank (13) through a pipeline.
3. The production system of the nizatidine skeleton raw material dimethylamino thioacetyl according to claim 1, characterized in that: and the dimethylamino acetonitrile reaction kettle (2) is connected with a low boiling tank (14) and a dimethylamino acetonitrile storage tank (15) in parallel through pipelines.
4. The production system of the nizatidine skeleton raw material dimethylamino thioacetyl according to claim 1, characterized in that: the front end of the sodium cyanide head tank (8) is connected with a sodium cyanide aqueous solution tank (16) through a pipeline.
5. The production system of the nizatidine skeleton raw material dimethylamino thioacetyl according to claim 1, characterized in that: the dimethylamino thioacetamide synthesis kettle (4) is connected with a first condenser (17) through a pipeline.
6. The production system of the nizatidine skeleton raw material dimethylamino thioacetyl according to claim 1, characterized in that: and the crystallization kettle (7) is connected with a second condenser (18) through a pipeline.
7. The system for producing raw material dimethylamino thioacetyl as nizatidine skeleton according to claim 1, characterized in that: and the toluene distillation kettle (11) is connected with a third condenser (19) through a pipeline.
8. The production system of claim 3, wherein the raw material of nizatidine skeleton is dimethylamino thioacetyl, and the production system is characterized in that: and a fourth condenser (20) is arranged on a pipeline between the dimethylamino acetonitrile reaction kettle (2) and the low-boiling tank (14).
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