CN118005568A - Processing technique and device for preparing acipimox - Google Patents
Processing technique and device for preparing acipimox Download PDFInfo
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- CN118005568A CN118005568A CN202311776543.8A CN202311776543A CN118005568A CN 118005568 A CN118005568 A CN 118005568A CN 202311776543 A CN202311776543 A CN 202311776543A CN 118005568 A CN118005568 A CN 118005568A
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- acipimox
- air
- drying
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- preparing
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- DJQOOSBJCLSSEY-UHFFFAOYSA-N Acipimox Chemical compound CC1=CN=C(C(O)=O)C=[N+]1[O-] DJQOOSBJCLSSEY-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229960003526 acipimox Drugs 0.000 title claims abstract description 54
- 238000012545 processing Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims description 16
- 238000001035 drying Methods 0.000 claims abstract description 75
- 238000007789 sealing Methods 0.000 claims abstract description 67
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 31
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960000583 acetic acid Drugs 0.000 claims abstract description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000002829 reductive effect Effects 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- LCZUOKDVTBMCMX-UHFFFAOYSA-N 2,5-Dimethylpyrazine Chemical compound CC1=CN=C(C)C=N1 LCZUOKDVTBMCMX-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 8
- 239000003814 drug Substances 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000001934 2,5-dimethylpyrazine Substances 0.000 claims abstract description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 239000001632 sodium acetate Substances 0.000 claims abstract description 4
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 4
- 230000002378 acidificating effect Effects 0.000 claims abstract description 3
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 38
- 238000000605 extraction Methods 0.000 claims description 30
- 238000001514 detection method Methods 0.000 claims description 26
- 239000012528 membrane Substances 0.000 claims description 22
- 230000009471 action Effects 0.000 claims description 9
- 238000011161 development Methods 0.000 claims description 8
- 230000006835 compression Effects 0.000 claims description 5
- 238000007906 compression Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000696 magnetic material Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 229940079593 drug Drugs 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000003672 processing method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- 230000018109 developmental process Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 208000031226 Hyperlipidaemia Diseases 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 201000005569 Gout Diseases 0.000 description 1
- 108010010234 HDL Lipoproteins Proteins 0.000 description 1
- 102000015779 HDL Lipoproteins Human genes 0.000 description 1
- 208000035150 Hypercholesterolemia Diseases 0.000 description 1
- 108010007622 LDL Lipoproteins Proteins 0.000 description 1
- 102000007330 LDL Lipoproteins Human genes 0.000 description 1
- 108010062497 VLDL Lipoproteins Proteins 0.000 description 1
- 210000000577 adipose tissue Anatomy 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003524 antilipemic agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 208000020346 hyperlipoproteinemia Diseases 0.000 description 1
- 208000006575 hypertriglyceridemia Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000029226 lipidation Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 210000002381 plasma Anatomy 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Drying Of Solid Materials (AREA)
Abstract
The invention relates to the technical field of pharmaceutical chemistry, in particular to a processing method and a processing device for preparing acipimox, comprising the following steps of oxidizing 2, 5-dimethyl pyrazine with hydrogen peroxide and glacial acetic acid for reaction, and extracting with an organic solvent to obtain an intermediate 1; refluxing the intermediate 1 and acetic acid in glacial acetic acid by using sodium acetate catalysis, and then distilling under reduced pressure to obtain an intermediate 2; hydrolyzing the intermediate 2 under alkaline condition, extracting with ethyl acetate and concentrating to obtain an intermediate 3; intermediate 3 was oxidized under acidic conditions, then extracted with butanone and distilled under reduced pressure to afford intermediate 4. The sealing device has the beneficial effects that the sealing state of the sealing strip can be detected when the sealing device is in a working state, and when the sealing strip is damaged or aged, the sealing effect is poor, and at the moment, the sealing device is started, so that the deformed sealing layer deforms and expands to form a second sealing layer, the outside air is isolated, and the quality of medicine drying is ensured.
Description
Technical Field
The invention relates to the technical field of pharmaceutical chemistry, in particular to a processing technique method and a processing device for preparing acipimox.
Background
Acipimox (Acipimox) is a new lipid-lowering drug for resisting lipidation, and can reduce the release of free fatty acid and the synthesis of triacylglycerol by inhibiting the decomposition of adipose tissues, so as to reduce the contents of total cholesterol, triglyceride, low-density lipoprotein and very low-density lipoprotein in blood plasma, improve the content of high-density lipoprotein and ensure durable and stable effect. Especially has good curative effect on patients with hyperlipidemia accompanied with gout and diabetes. Is mainly used for treating hypertriglyceridemia (IV type), hypercholesterolemia IIa type and IIb type, III type and V type hyperlipoproteinemia.
The acipimox needs to be dried in the preparation process, so that moisture and solvent in the acipimox are removed, the purity and stability of the acipimox are improved, but in the use process of an existing drying box, the sealing of the box body and a cabinet door is realized through sealing strips, the sealing strips can be aged, deformed, fallen or damaged along with the time, the sealing effect is reduced, moisture in the outside air enters the drying box, the moisture content of the acipimox is increased, and the purity and stability of the acipimox are influenced.
Disclosure of Invention
Some simplifications or omissions may be made in this section as well as in the description of the application and in the title of the application, which may not be used to limit the scope of the application.
The invention aims to provide a processing technology method for preparing acipimox.
Therefore, the object is to solve: the sealing strip may be aged, deformed, fallen or damaged over time, and the sealing effect is reduced, so that moisture in the outside air enters the drying box.
In order to solve the technical problems, the invention provides the following technical scheme: a processing technology method for preparing acipimox comprises the following steps of oxidizing 2, 5-dimethyl pyrazine with hydrogen peroxide and glacial acetic acid for reaction, and then extracting with an organic solvent to obtain an intermediate 1;
refluxing the intermediate 1 and acetic acid in glacial acetic acid by using sodium acetate catalysis, and then distilling under reduced pressure to obtain an intermediate 2;
hydrolyzing the intermediate 2 under alkaline condition, extracting with ethyl acetate and concentrating to obtain an intermediate 3;
Oxidizing the intermediate 3 under an acidic condition, extracting with butanone, and distilling under reduced pressure to obtain an intermediate 4;
Reacting the intermediate 4 under the action of sodium tungstate and hydrogen peroxide, and then carrying out suction filtration and putting the reaction product into a drying device to obtain a crude acipimox product;
the drying device detects self sealing performance in the drying process so as to ensure the drying quality.
The processing device for preparing the acipimox has the beneficial effects that: the sealing state of the sealing strip can be detected when the detection plugging device is in a working state, when the sealing strip is damaged or ageing problems occur, the sealing effect is poor, so that external gas can enter the detection port when in the working state, at the moment, the detection plugging device is started, and the deformation sealing layer is deformed and expanded to form a second sealing layer so as to isolate external air and ensure the quality of medicine drying.
In view of the fact that in the actual use process, the problem that the passive piston cannot reset due to gas entering the passive piston exists.
In order to solve the technical problems, the invention also provides the following technical scheme: the processing device for preparing the acipimox comprises the processing technology method for preparing the acipimox, and further comprises a drying device, wherein the drying device comprises a drying box, a drying cavity for drying medicines is arranged in the drying box, a cabinet door is arranged on one side of the drying cavity and used for sealing the drying cavity, and a sealing strip is fixed on one side of the cabinet door facing the drying cavity; the extraction device comprises an air extraction cylinder body arranged in the drying box, a lifting piece arranged below the air extraction cylinder body, a driving piece arranged below the lifting piece and used for driving the lifting piece to operate, and a gas conveying pipe used for extracting wet gas during drying; and the detection plugging device is arranged on the outer side of the air extraction cylinder body and is used for detecting the sealing performance of the cabinet door.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the lifting piece comprises a lifting rod which movably penetrates through the bottom of the air extraction cylinder body, a lifting piston is fixedly arranged on the top of the lifting rod, a supporting cylinder body is sleeved on the part, located outside the air extraction cylinder body, of the lifting rod in a sliding mode, and the supporting cylinder body is fixed on the drying box.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the driving piece is including being fixed in the guide board of lifter bottom, guide board one side is equipped with the cam, the cam outside is fixed with the drive block, guide board inside has been seted up and has been held the gliding drive slot of drive block, one side transmission that the guide board was kept away from to the cam is connected with the motor.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the air conveying pipe comprises a first air inlet pipe and a first air outlet pipe which are respectively communicated with the air suction barrel, one end of the first air inlet pipe, which is far away from the air suction barrel, is communicated with the drying cavity, one end of the first air outlet pipe, which is far away from the air suction barrel, is communicated with the outside, and first unidirectional elastic diaphragms for controlling the air flowing direction are arranged in the first air inlet pipe and the first air outlet pipe; the first unidirectional elastic membrane comprises a fixed ring and a membrane, and the edge of the membrane part is fixed on the fixed ring.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the detection plugging device comprises a sleeve fixed on the outer side of the air extraction cylinder body, a passive piston is connected inside the sleeve in a sliding mode, and magnetic materials are contained inside the passive piston and the lifting piston.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the detection plugging device further comprises a second air inlet pipe and a second air outlet pipe which are respectively communicated with the sleeve, and a detection port which is formed in the outer side of the drying box and corresponds to the sealing strip, wherein one end of the second air inlet pipe, which is far away from the sleeve, is communicated with the detection port, the sealing strip is further fixed with a deformation sealing layer towards one side of the drying cavity, one end of the second air outlet pipe, which is far away from the sleeve, is communicated with the deformation sealing layer, and second unidirectional elastic diaphragms are arranged in the second air outlet pipe and the second air inlet pipe so as to control the flow direction of gas.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the outer side of the sleeve is provided with a resetting device for resetting the passive piston, the resetting device comprises a resetting ring which is arranged on the outer side of the sleeve in a sliding manner, and the inner wall of the resetting ring is fixedly provided with a magnetic sheet for magnetically attracting the passive piston; wherein, the sleeve upper half is fixed with the magnetic shielding board.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the sleeve is characterized in that a guide groove for guiding the reset ring to slide is formed in the outer side of the sleeve, a compression spring which plays a role in abutting the reset ring is arranged in the guide groove, and an exhaust hole corresponding to the reset ring is formed in the upper half part of the sleeve.
As a preferred embodiment of the processing apparatus for preparing acipimox according to the present invention, wherein: the drying box surface is provided with color development device for remind the cabinet door that loses sealing performance, color development device is including being fixed in the observation window on the drying box, the observation window is inside to be fixed with the layer that discolours, one side that the observation window was kept away from to the layer that discolours is fixed with the pressurized layer, it has pressurized solution to pack between pressurized layer and the layer that discolours, pressurized layer part is located the second outlet duct.
The processing device for preparing the acipimox has the beneficial effects that: the reset ring drives the passive piston to move upwards through the magnetic force generated by the magnetic sheet, and the lifting height of the passive piston is limited through the magnetic shielding plate made of the magnetic shielding material, so that the influence of the magnetic force of the magnetic sheet is isolated under the action of the magnetic shielding plate, the magnetic force parts are prevented from interfering with each other, the passive piston can stay at a preset height, and redundant gas in the reset ring is discharged from the exhaust hole so as to be reused.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
fig. 1 is a flow chart of a process for preparing acipimox according to the present invention.
Fig. 2 is a schematic perspective view of a processing device for preparing acipimox according to the present invention.
Fig. 3 is a schematic front view of the processing device for preparing acipimox according to the present invention.
Fig. 4 is a schematic cross-sectional structural diagram of an air extraction cylinder of a processing device for preparing acipimox in the invention.
Fig. 5 is a schematic perspective view of a first unidirectional elastic membrane of the processing device for preparing acipimox according to the present invention.
Fig. 6 is a schematic cross-sectional structure of a sleeve of a processing device for preparing acipimox according to the present invention.
Fig. 7 is a schematic perspective view of a reset device of the processing device for preparing acipimox in the present invention.
FIG. 8 is a schematic diagram showing the sectional structure of a color development device of a processing device for preparing acipimox in the present invention.
In the figure:
100. A drying device; 101. a drying box; 102. a cabinet door; 103. a sealing strip;
200. Extraction means; 201. an air extraction cylinder; 202. a lifting member; 203. a driving member; 204. a gas delivery tube; 205. a first unidirectional elastic membrane;
202a, lifting rod; 202b, lifting the piston;
203a, a guide plate; 203b, a cam;
204a, a first air inlet pipe; 204b, a first air outlet pipe;
205a, a fixing ring; 205b, a diaphragm;
300. detecting a plugging device; 301. a sleeve; 302. a passive piston; 303. a second air inlet pipe; 304. a second air outlet pipe; 305. a second unidirectional elastic membrane;
303a, a detection port;
304a, a deformable sealing layer;
400. A reset device; 401. a reset ring; 402. a magnetic sheet; 403. a guide groove; 404. a compression spring; 405. a magnetic shield panel;
401a, exhaust holes;
500. a color development device; 501. an observation window; 502. a pressed layer; 503. the solution is pressurized.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Referring to FIG. 1, a first embodiment of the present invention provides a process for preparing acipimox, comprising the steps of
2, 5-Dimethyl pyrazine, hydrogen peroxide and glacial acetic acid are put into a reaction kettle, the mass ratio of the three substances is 1:2:5, the reaction temperature is 70-80 ℃, and the reaction time is 10-14 hours. Evaporating acetic acid under reduced pressure after the reaction is completed, adding alkali to adjust the pH value to be more than 10, extracting by using an organic solvent, evaporating the solvent after drying, and recrystallizing residues by using benzene or toluene to obtain an intermediate 1;
Adding glacial acetic acid (solvent), acetic acid, sodium acetate (catalyst) and the intermediate 1 into a reaction kettle, carrying out reflux reaction for 4-7 hours, evaporating the solvent under reduced pressure, and collecting 120 ℃/12mg of hexaplite as the intermediate 2;
Adding the intermediate 2 into 10% sodium hydroxide solution, stirring at room temperature for reaction for 24 hours, extracting with ethyl acetate, drying and concentrating to obtain an intermediate 3;
Dissolving the intermediate 3 in water, dripping a potassium permanganate aqueous solution under stirring, reacting for 1 hour, adding hydrochloric acid to enable the purple of the solution to disappear, filtering, extracting filtrate with butanone, drying, and evaporating the solvent under reduced pressure to obtain an intermediate 4;
Adding sodium tungstate (catalyst) and 30% hydrogen peroxide into water, adjusting pH to be 1.5, adding an intermediate 4, reacting at 70 ℃ for 14-16 seconds to disappear, cooling, suction filtering, and drying to obtain a crude acipimox product;
the drying device 100 detects its sealing property during the drying process to ensure the drying quality.
Example 2
Referring to fig. 2 to 3, in a second embodiment of the present invention, unlike the previous embodiment, a processing apparatus for preparing acipimox includes a processing method for preparing acipimox, and further includes a drying apparatus 100 including a drying box 101, a drying chamber for drying a medicine is provided in the drying box 101, a cabinet door 102 is provided at one side of the drying chamber for sealing the drying chamber, and a sealing strip 103 is fixed at one side of the cabinet door 102 facing the drying chamber; the stoving case 101 need be with cabinet door 102 when drying acipimox, realizes sealedly through extrusion sealing strip 103 when cabinet door 102 is closed, effectively prevents that the steam in the outside air from being absorbed by acipimox when drying, causes the problem of quality decline.
The extraction device 200 comprises an air extraction cylinder 201 arranged in the drying box 101, a lifting piece 202 arranged below the air extraction cylinder 201, a driving piece 203 arranged below the lifting piece 202 and used for driving the lifting piece 202 to operate, and a gas conveying pipe 204 used for extracting moist gas during drying; the detection plugging device 300 is arranged outside the air extraction cylinder 201 and is used for detecting the sealing performance of the cabinet door 102.
Further, the lifting member 202 includes a lifting rod 202a movably penetrating through the bottom of the air extraction cylinder 201, a lifting piston 202b is fixedly installed on the top of the lifting rod 202a at a portion of the air extraction cylinder 201, a supporting cylinder is slidably sleeved on a portion of the lifting rod 202a at the outer side of the air extraction cylinder 201, and the supporting cylinder is fixed on the drying box 101. Referring to fig. 3 to 4, the lifting rod 202a may push and pull the lifting piston 202b to move up and down, when the lifting piston 202b is lifted, the gas above is extruded to be discharged, when the lifting piston 202b is lowered, the internal air pressure is reduced to form negative pressure, so that the gas can be extracted, the wet gas in the drying box can be extracted in a reciprocating and sustainable manner, the drying effect is ensured, the drying box 101 is internally provided with an air inlet to supplement the normal flow of the internal gas, and a filtering device, such as an activated carbon layer, is arranged at the air inlet to filter the vapor and impurities in the gas, so as to prevent pollution; the supporting cylinder body plays a role in supporting the sliding of the lifting rod 202a, so that the lifting rod 202a is more stable when sliding in a reciprocating manner.
The driving piece 203 comprises a guide plate 203a fixed at the bottom of the lifting rod 202a, a cam 203b is arranged on one side of the guide plate 203a, a driving block is fixed on the outer side of the cam 203b, a driving groove for accommodating the sliding of the driving block is formed in the guide plate 203a, and one side, far away from the guide plate 203a, of the cam 203b is in transmission connection with a motor. Referring to fig. 4, when the motor works, the cam 203b is driven to continuously rotate, the driving block of the cam 203b slides back and forth in the driving groove and pushes the guiding plate 203a to move up and down during the rotation, and the lifting rod 202a is fixed on the top of the guiding plate 203a, so that the lifting rod 202a is synchronously driven to move up and down, and the lifting rod 202a drives the lifting piston 202b to reciprocate for exhausting.
The gas conveying pipe 204 comprises a first gas inlet pipe 204a and a first gas outlet pipe 204b which are respectively communicated with the gas extraction cylinder 201, one end of the first gas inlet pipe 204a, which is far away from the gas extraction cylinder 201, is communicated with a drying cavity, one end of the first gas outlet pipe 204b, which is far away from the gas extraction cylinder 201, is communicated with the outside, and first unidirectional elastic diaphragms 205 for controlling the gas flow direction are arranged in the first gas inlet pipe 204a and the first gas outlet pipe 204 b; wherein the first unidirectional elastic diaphragm 205 includes a fixed ring 205a and a diaphragm 205b, and a portion of the edge of the diaphragm 205b is fixed on the fixed ring 205 a. Referring to fig. 3 to 5, when the lifting piston 202b descends, the internal air pressure becomes smaller, so that the first unidirectional elastic membrane 205 at the first air inlet pipe 204a is opened under the action of air pressure, the first unidirectional elastic membrane 205 at the first air outlet pipe 204b is closed under the action of air pressure, so that the wet air in the drying cavity can be extracted through the first air inlet pipe 204a, when the lifting piston 202b ascends, the internal air pressure is extruded to become larger, so that the first unidirectional elastic membrane 205 at the first air inlet pipe 204a is closed under the action of air pressure, the first unidirectional elastic membrane 205 at the first air outlet pipe 204b is opened under the action of air pressure, so that the wet air is discharged from the first air outlet pipe 204b, and the continuous discharge of the wet air is realized, thereby replacing the air pump to work, and the extraction device 200 can drive the detection plugging device 300 to operate during work, so that the structure is more compact, and excessive electrical equipment is not required to be added.
Referring to fig. 4 to 5, in addition, the fixing ring 205a is fixed to the inner wall of the gas delivery pipe 204, and the diaphragm 205b is made of an elastic rubber material and attached to one side of the fixing ring 205a, so that the diaphragm 205b is opened when the pressure generated by the gas pressure overcomes the deformation force of the diaphragm 205b, thereby allowing the gas to pass therethrough, and when the gas flows back, the pressure generated by the gas can make the attachment of the diaphragm 205b and the fixing ring 205a tighter, thereby realizing unidirectional passage of the gas, that is, by changing the installation positions of the two diaphragms 205b, the direction of the gas flow can be controlled.
Example 3
Referring to fig. 2-5, a third embodiment of the present invention further provides a processing apparatus for preparing acipimox. The detection plugging device 300 comprises a sleeve 301 fixed on the outer side of the air extraction cylinder 201, a passive piston 302 is connected inside the sleeve 301 in a sliding manner, and the passive piston 302 and the lifting piston 202b both contain magnetic materials. The magnetic materials contained in the passive piston 302 and the lifting piston 202b can be strong magnets, so that the magnetic force generated by the lifting piston 202b on the passive piston 302 in the moving process overcomes the friction force of the passive piston 302 to drive the passive piston 302 to synchronously move, wherein rubber is wrapped on the outer sides of the passive piston 302 and the lifting piston 202b, and the gas can be pushed in the moving process.
The detection plugging device 300 further comprises a second air inlet pipe 303 and a second air outlet pipe 304 which are respectively communicated with the sleeve 301, and a detection port 303a which is formed in the outer side of the drying box 101 and corresponds to the sealing strip 103, one end, away from the sleeve 301, of the second air inlet pipe 303 is communicated with the detection port 303a, the sealing strip 103 is further fixed with a deformation sealing layer 304a on one side, facing the drying cavity, of the sealing strip 103, one end, away from the sleeve 301, of the second air outlet pipe 304 is communicated with the deformation sealing layer 304a, and second unidirectional elastic diaphragms 305 are respectively arranged in the second air outlet pipe 304 and the second air inlet pipe 303 so as to control the air flow direction. Referring to fig. 2 and fig. 4-6, since the sealing strip 103 is attached to the detection port 303a when closed, the detection port 303a is sealed, the sleeve 301 is communicated with the detection port 303a through the second air inlet pipe 303, at this time, the air pressure inside the sleeve 301 is in an equilibrium state, the acting force generated by the air pressure is greater than the magnetic force, so the passive piston 302 cannot move along with the lifting piston 202b, it is to be noted that the second unidirectional elastic membrane 305 is installed inside the second unidirectional elastic membrane 305 and the second air outlet pipe 304, and the structure of the second unidirectional elastic membrane 305 is the same as that of the first unidirectional elastic membrane 205, so that the flowing direction of the air can be controlled;
When the sealing strip 103 is damaged or aged, the sealing effect is poor, so that the external air can enter the detection port 303a in the working state, and the air pressure balance is broken, at this time, referring to fig. 5, when the lifting piston 202b moves downwards, the magnetic force generated by the lifting piston is used to drive the passive piston 302 to move downwards, the negative pressure generated in the downward moving process opens the second unidirectional elastic membrane 305 at the second air inlet pipe 303, the second unidirectional elastic membrane 305 at the second air outlet pipe 304 is closed under the action of the negative pressure, so that the air at the detection port 303a can be singly extracted, when the passive piston 302 is lifted by the lifting piston 202b, at this time, the second unidirectional elastic membrane 305 at the second air inlet pipe 303 is in the closed state under the action of the air pressure, and the second unidirectional elastic membrane 305 at the second air outlet pipe 304 is in the open state, so that the extracted air is conveyed into the deformed sealing layer 304a through the second air outlet pipe 304, the deformed sealing layer 304a is made of an elastic material, and under the condition that the air is continuously conveyed by the detection plugging device 300, the deformed and expanded to form the second sealing layer, and the quality of the dried sealing layer is ensured.
Example 4
Referring to fig. 5-8, a third embodiment of the present invention further provides a processing apparatus for preparing acipimox. The device comprises a reset device 400 arranged on the outer side of a sleeve 301 and used for resetting a passive piston 302, wherein the reset device 400 comprises a reset ring 401 arranged on the outer side of the sleeve 301 in a sliding manner, and a magnetic sheet 402 of the magnetic passive piston 302 is fixed on the inner wall of the reset ring 401; wherein the upper half of the sleeve 301 is fixed with a magnetic shield panel 405. A guide groove 403 for guiding the reset ring 401 to slide is formed on the outer side of the sleeve 301, a compression spring 404 for abutting the reset ring 401 is mounted in the guide groove 403, and an exhaust hole 401a corresponding to the reset ring 401 is formed in the upper half of the sleeve 301. Referring to fig. 6-7, after the passive piston 302 is triggered, part of gas remains inside, so when the sealing effect of the sealing strip 103 is poor, the passive piston 302 will not cause the deformation sealing layer 304a to expand by mistake because the redundant gas inside the sleeve 301 is not discharged, and the service life of the sealing strip is affected, so after each time the sealing strip 103 is replaced, a worker needs to push the reset ring 401 down to the bottom manually, the reset ring 401 drives the passive piston 302 to move upwards through the magnetic force generated by the magnetic sheet 402, and the lifting height of the passive piston 302 is limited through the magnetic shielding plate 405 made of the magnetic shielding material, the influence of the magnetic force of the magnetic sheet 402 is isolated under the effect of the magnetic shielding plate 405, so that the magnetic force components are prevented from interfering with each other, and the passive piston 302 will stay at a preset height, so that the redundant gas in the reset ring 401 is discharged from the exhaust hole 401a, and the reset ring 401 is fixed with a sealing pad corresponding to the exhaust hole 401a, so as to avoid air leakage.
The guiding groove 403 is vertically formed on the sleeve 301, so that the sliding of the reset ring 401 is smoother, and the reset ring 401 is applied with upward thrust through the compression spring 404, so that the reset ring 401 cannot slide down by mistake to affect the normal operation of the passive piston 302.
The stoving case 101 surface is provided with color rendering device 500 for remind cabinet door 102 that loses sealing performance, color rendering device 500 is fixed with the color change layer including being fixed in the observation window 501 on the stoving case 101, and the one side that the observation window 501 was kept away from to the color change layer is fixed with pressurized layer 502, and pressurized solution 503 is filled between pressurized layer 502 and the color change layer, and pressurized layer 502 part is arranged in second outlet duct 304. Referring to fig. 5-7, when the second air outlet pipe 304 is supplied with air, the air is blocked by the pressure-receiving layer 502, the pressure-receiving layer 502 is an elastic rubber layer, when the pressure generated in the second air outlet pipe 304 is greater than the deformation force of the pressure-receiving layer 502, the pressure-receiving layer 502 is compressed, the pressure-receiving layer 502 transmits the force to the color-changing layer through the pressure-receiving solution 503, and the color-changing layer is made of pressure-changing color-changing material, such as liquid crystal, so that the staff is reminded of the decrease of the sealing performance of the sealing strip 103 through the change of color, and the replacement is needed in time.
It is important to note that the construction and arrangement of the application as shown in the various exemplary embodiments is illustrative only. Although only a few embodiments have been described in detail in this disclosure, those skilled in the art who review this disclosure will readily appreciate that many modifications are possible (e.g., variations in sizes, dimensions, structures, shapes and proportions of the various elements, values of parameters (e.g., temperature, pressure, etc.), mounting arrangements, use of materials, colors, orientations, etc.) without materially departing from the novel teachings and advantages of the subject matter described in this application. For example, elements shown as integrally formed may be constructed of multiple parts or elements, the position of elements may be reversed or otherwise varied, and the nature or number of discrete elements or positions may be altered or varied. Accordingly, all such modifications are intended to be included within the scope of present application. The order or sequence of any process or method steps may be varied or re-sequenced according to alternative embodiments. In the claims, any means-plus-function clause is intended to cover the structures described herein as performing the recited function and not only structural equivalents but also equivalent structures. Other substitutions, modifications, changes and omissions may be made in the design, operating conditions and arrangement of the exemplary embodiments without departing from the scope of the present applications. Therefore, the application is not limited to the specific embodiments, but extends to various modifications that nevertheless fall within the scope of the appended claims.
Furthermore, in order to provide a concise description of the exemplary embodiments, all features of an actual implementation may not be described (i.e., those not associated with the best mode presently contemplated for carrying out the invention, or those not associated with practicing the invention).
It should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation-specific decisions may be made. Such a development effort might be complex and time consuming, but would nevertheless be a routine undertaking of design, fabrication, and manufacture for those of ordinary skill having the benefit of this disclosure.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (10)
1. A processing technique for preparing acipimox is characterized in that: comprises the following steps of the method,
Oxidizing 2, 5-dimethyl pyrazine with hydrogen peroxide and glacial acetic acid for reaction, and extracting with an organic solvent to obtain an intermediate 1;
refluxing the intermediate 1 and acetic acid in glacial acetic acid by using sodium acetate catalysis, and then distilling under reduced pressure to obtain an intermediate 2;
hydrolyzing the intermediate 2 under alkaline condition, extracting with ethyl acetate and concentrating to obtain an intermediate 3;
Oxidizing the intermediate 3 under an acidic condition, extracting with butanone, and distilling under reduced pressure to obtain an intermediate 4;
Reacting the intermediate 4 under the action of sodium tungstate and hydrogen peroxide, and then carrying out suction filtration and putting the reaction product into a drying device to obtain a crude acipimox product;
the drying device detects self sealing performance in the drying process so as to ensure the drying quality.
2. A processing device for preparing acipimox, which is characterized in that: the process for preparing acipimox according to claim 1, which comprises,
The drying device (100) comprises a drying box (101), a drying cavity for drying the medicines is arranged in the drying box (101), a cabinet door (102) is arranged on one side of the drying cavity and used for sealing the drying cavity, and a sealing strip (103) is fixed on one side, facing the drying cavity, of the cabinet door (102);
The extraction device (200) comprises an air extraction cylinder (201) arranged in the drying box (101), a lifting piece (202) arranged below the air extraction cylinder (201), a driving piece (203) arranged below the lifting piece (202) and used for driving the lifting piece (202) to operate, and a gas conveying pipe (204) used for extracting humid gas during drying;
And the detection plugging device (300) is arranged outside the air extraction cylinder (201) and is used for detecting the sealing performance of the cabinet door (102).
3. The processing apparatus for preparing acipimox according to claim 2, wherein: the lifting piece (202) comprises a lifting rod (202 a) which movably penetrates through the bottom of the air extraction cylinder (201), a lifting piston (202 b) is fixedly arranged at the top of the lifting rod (202 a) and positioned on the air extraction cylinder (201), a supporting cylinder is sleeved on the part, positioned outside the air extraction cylinder (201), of the lifting rod (202 a) in a sliding mode, and the supporting cylinder is fixed on the drying box (101).
4. A processing apparatus for the preparation of acipimox as claimed in claim 3, wherein: the driving piece (203) comprises a guide plate (203 a) fixed at the bottom of the lifting rod (202 a), a cam (203 b) is arranged on one side of the guide plate (203 a), a driving block is fixed on the outer side of the cam (203 b), a driving groove for accommodating the driving block to slide is formed in the guide plate (203 a), and a motor is connected to one side of the cam (203 b) far away from the guide plate (203 a) in a transmission manner.
5. The processing device for preparing acipimox according to claim 4, wherein: the air conveying pipe (204) comprises a first air inlet pipe (204 a) and a first air outlet pipe (204 b) which are respectively communicated with the air suction cylinder (201), one end, away from the air suction cylinder (201), of the first air inlet pipe (204 a) is communicated with the drying cavity, one end, away from the air suction cylinder (201), of the first air outlet pipe (204 b) is communicated with the outside, and first unidirectional elastic diaphragms (205) for controlling the air flow direction are arranged in the first air inlet pipe (204 a) and the first air outlet pipe (204 b); the first unidirectional elastic membrane (205) comprises a fixed ring (205 a) and a membrane (205 b), and part of the edge of the membrane (205 b) is fixed on the fixed ring (205 a).
6. A processing apparatus for the preparation of acipimox as claimed in claim 3, wherein: the detection plugging device (300) comprises a sleeve (301) fixed on the outer side of the air extraction cylinder body (201), a passive piston (302) is connected inside the sleeve (301) in a sliding mode, and magnetic materials are contained inside the passive piston (302) and the lifting piston (202 b).
7. The processing apparatus for preparing acipimox according to claim 6, wherein: the detection plugging device (300) further comprises a second air inlet pipe (303) and a second air outlet pipe (304) which are respectively communicated with the sleeve (301), and a detection port (303 a) which is arranged on the outer side of the drying box (101) and corresponds to the sealing strip (103), one end, away from the sleeve (301), of the second air inlet pipe (303) is communicated with the detection port (303 a), a deformation sealing layer (304 a) is further fixed on one side, facing the drying cavity, of the sealing strip (103), one end, away from the sleeve (301), of the second air outlet pipe (304) is communicated with the deformation sealing layer (304 a), and second unidirectional elastic membranes (305) are respectively arranged inside the second air outlet pipe (304) and the second air inlet pipe (303) so as to control the air flow direction.
8. The processing apparatus for preparing acipimox according to claim 7, wherein: a reset device (400) is arranged on the outer side of the sleeve (301) and used for resetting the passive piston (302), the reset device (400) comprises a reset ring (401) which is arranged on the outer side of the sleeve (301) in a sliding manner, and a magnetic sheet (402) of the magnetic passive piston (302) is fixed on the inner wall of the reset ring (401); wherein, a magnetic shielding plate (405) is fixed on the upper half part of the sleeve (301).
9. The processing apparatus for preparing acipimox according to claim 8, wherein: the sleeve (301) is provided with a guide groove (403) for guiding the reset ring (401) to slide, a compression spring (404) which is used for abutting the reset ring (401) is arranged in the guide groove (403), and the upper half part of the sleeve (301) is provided with an exhaust hole (401 a) corresponding to the reset ring (401).
10. The processing apparatus for preparing acipimox according to claim 6, wherein: the drying box (101) surface is provided with color development device (500) for remind cabinet door (102) that lose sealing performance, color development device (500) are including being fixed in observation window (501) on drying box (101), observation window (501) inside is fixed with the layer that discolours, and one side that observation window (501) was kept away from to the layer that discolours is fixed with pressurized layer (502), it has pressurized solution (503) to fill between pressurized layer (502) and the layer that discolours, pressurized layer (502) part is located second outlet duct (304).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311776543.8A CN118005568A (en) | 2023-12-22 | 2023-12-22 | Processing technique and device for preparing acipimox |
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| CN202311776543.8A CN118005568A (en) | 2023-12-22 | 2023-12-22 | Processing technique and device for preparing acipimox |
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| CN116952485A (en) * | 2023-07-27 | 2023-10-27 | 上海云懋空气处理设备有限公司 | Sealing performance detection device, rotary dehumidifier and sealing performance detection method |
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