CN211570508U - Hydrogenation reaction system for valaciclovir hydrochloride production - Google Patents
Hydrogenation reaction system for valaciclovir hydrochloride production Download PDFInfo
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- CN211570508U CN211570508U CN201922367462.8U CN201922367462U CN211570508U CN 211570508 U CN211570508 U CN 211570508U CN 201922367462 U CN201922367462 U CN 201922367462U CN 211570508 U CN211570508 U CN 211570508U
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- hydrogenation
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- reaction system
- hydrogenation reaction
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- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- ZCDDBUOENGJMLV-QRPNPIFTSA-N Valacyclovir hydrochloride Chemical compound Cl.N1C(N)=NC(=O)C2=C1N(COCCOC(=O)[C@@H](N)C(C)C)C=N2 ZCDDBUOENGJMLV-QRPNPIFTSA-N 0.000 title claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 238000002425 crystallisation Methods 0.000 claims abstract description 16
- 230000008025 crystallization Effects 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 229940064636 valacyclovir hydrochloride Drugs 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 8
- 239000002893 slag Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010079 rubber tapping Methods 0.000 claims description 3
- HDOVUKNUBWVHOX-QMMMGPOBSA-N Valacyclovir Chemical compound N1C(N)=NC(=O)C2=C1N(COCCOC(=O)[C@@H](N)C(C)C)C=N2 HDOVUKNUBWVHOX-QMMMGPOBSA-N 0.000 claims description 2
- 229940093257 valacyclovir Drugs 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 21
- 238000009833 condensation Methods 0.000 abstract description 9
- 230000005494 condensation Effects 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 5
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229960004150 aciclovir Drugs 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- MKUXAQIIEYXACX-UHFFFAOYSA-N aciclovir Chemical compound N1C(N)=NC(=O)C2=C1N(COCCO)C=N2 MKUXAQIIEYXACX-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- 208000007514 Herpes zoster Diseases 0.000 description 1
- 208000029433 Herpesviridae infectious disease Diseases 0.000 description 1
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-Valine Natural products CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 description 1
- 125000003580 L-valyl group Chemical group [H]N([H])[C@]([H])(C(=O)[*])C(C([H])([H])[H])(C([H])([H])[H])[H] 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 229940002612 prodrug Drugs 0.000 description 1
- 239000000651 prodrug Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229960004295 valine Drugs 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The hydrogenation reaction system for valaciclovir hydrochloride production comprises a hydrogenation bin, wherein a first feeding pipe is arranged at the top of the hydrogenation bin, a motor is arranged at the top of the hydrogenation bin, a shaft of the motor vertically penetrates downwards into the hydrogenation bin and is connected with a rotating shaft arranged in the hydrogenation bin through a coupling, a U-shaped stirring frame is arranged on the rotating shaft and is attached to the bottom and the side wall of the hydrogenation bin; a second feeding pipe, an air inlet pipe and an air return pipe are arranged on the side wall of the hydrogenation bin; the bottom of the hydrogenation bin is connected with the filtering bin through a liquid feeding pipe, and the filtering bin is connected with the crystallization bin through a connecting pipe. By adopting the structure, the whole hydrogenation reaction process can be automatically completed, the solid condensation compound intermediate can be quickly dissolved in methanol, the time consumed by stirring and mixing can be shortened, and the production efficiency is improved.
Description
Technical Field
The utility model relates to a valaciclovir hydrochloride production field, it is specific that valaciclovir hydrochloride production is with hydrogenation reaction system.
Background
Valacyclovir hydrochloride is L-valine acid ester of acyclovir, is a prodrug of acyclovir, and is mainly used for treating herpes zoster and simple herpes virus infection of skin mucosa. Valaciclovir hydrochloride production mainly comprises two stages of esterification and hydrogenation, wherein the hydrogenation is carried out after a Pd/C catalyst and hydrogen are added into a condensation compound intermediate generated in the esterification, and because the tank body of a reaction tank is large, in the process of adding a methanol solution into a solid condensation compound, the blanking point of the solid condensation compound is fixed, so that full mixing and dissolution cannot be realized, the stirring time is long, and the reaction time is prolonged.
Disclosure of Invention
The utility model aims to solve the technical problem that a hydrogenation reaction system is used in valaciclovir hydrochloride production is provided, whole hydrogenation reaction flow can be accomplished automatically to realized that solid condensation thing midbody dissolves at the quick of methyl alcohol, can shorten the time that the stirring compounding needs to consume, improved production efficiency.
In order to solve the technical problem, the utility model discloses the technical scheme who adopts is: the hydrogenation reaction system for valaciclovir hydrochloride production comprises a hydrogenation bin, wherein a first feeding pipe is arranged at the top of the hydrogenation bin, a motor is arranged at the top of the hydrogenation bin, a shaft of the motor vertically penetrates downwards into the hydrogenation bin and is connected with a rotating shaft arranged in the hydrogenation bin through a coupling, a U-shaped stirring frame is arranged on the rotating shaft and is attached to the bottom and the side wall of the hydrogenation bin;
a second feeding pipe, an air inlet pipe and an air return pipe are arranged on the side wall of the hydrogenation bin;
the bottom of the hydrogenation bin is connected with a filtering bin through a liquid delivery pipe, and the filtering bin is connected with a crystallization bin through a connecting pipe.
In the preferred scheme, hydrogenation storehouse in still be equipped with the baffle on being close to the position at top, the equipartition is equipped with a plurality of unloading holes on the baffle, be equipped with the bearing on the baffle central point position, the bearing is passed in the pivot, be equipped with the strip in the pivot of baffle top and be the scraper blade of level setting, the bottom surface and the contact of baffle top surface of scraper blade.
In a preferred scheme, the number of the U-shaped stirring frames is two, the two U-shaped stirring frames are connected and fixed in a cross manner, and the lower end of the rotating shaft is fixedly arranged at the cross point of the two U-shaped stirring frames;
the rotating shaft is provided with a vertical plate which is positioned in the same vertical range with the vertical sections at the two sides of the U-shaped stirring frame.
In a preferable scheme, the air outlet end of the air inlet pipe is arranged in an area between the vertical plate and the vertical section of the U-shaped stirring frame.
In a preferable scheme, a slag tapping branch pipe is arranged on the liquid conveying pipe.
In the preferred scheme, the filter bin is provided with a negative pressure pump, and the side wall of the filter bin is also provided with a water inlet pipe.
In a preferred scheme, a first filter screen is arranged in the connecting pipe.
In the preferred scheme, an acetone pipe and an acetic acid pipe are arranged on the side wall of the crystallization bin, a recovery pipe is further arranged on the side wall of the crystallization bin at a position close to the bottom, and a second filter screen is arranged in the recovery pipe;
the bottom of the crystallization bin is provided with a discharge pipe.
The utility model provides a valaciclovir hydrochloride production is with hydrogenation reaction system through adopting above-mentioned structure, has following beneficial effect:
(1) the structure that the baffle plate is matched with the scraper plate is utilized, so that the blanking points of the solid condensation compound intermediate are uniformly distributed in the hydrogenation bin, the condensation compound intermediate and methanol can be fully mixed, the time consumption of mixing and dissolving is shortened, and the production efficiency is improved;
(2) the driving of the scraping plate and the stirring frame is realized by using a single motor, so that the whole driving structure is simpler;
(3) the method realizes one-step operation in the whole hydrogenation reaction process, and other operations are not required to be carried out manually in the reaction process.
Drawings
The invention will be further explained with reference to the following figures and examples:
fig. 1 is a schematic view of the overall overlooking structure of the present invention.
Fig. 2 is a schematic structural diagram of the stirring mechanism of the present invention.
Fig. 3 is a schematic diagram of the partition structure of the present invention.
In the figure: hydrogenation storehouse 1, first inlet pipe 2, baffle 3, unloading hole 301, bearing 302, scraper blade 4, motor 5, pivot 6, "U" shape stirring frame 7, riser 8, second inlet pipe 9, intake pipe 9', muffler 10, liquid delivery pipe 11, slag tap branch pipe 12, liquid delivery pump 13, filter storehouse 14, negative pressure pump 15, inlet tube 16, connecting pipe 17, first filter screen 171, crystallization storehouse 18, acetone pipe 19, recovery tube 20, second filter screen 2001, acetic acid pipe 21, discharging pipe 22.
Detailed Description
Example 1:
as shown in fig. 1-3, the hydrogenation reaction system for valacyclovir hydrochloride production comprises a hydrogenation chamber 1, wherein a first feeding pipe 2 is arranged at the top of the hydrogenation chamber 1, a motor 5 is arranged at the top of the hydrogenation chamber 1, the shaft of the motor 5 vertically penetrates downwards into the hydrogenation chamber 1 and is connected with a rotating shaft 6 arranged in the hydrogenation chamber 1 through a coupler, a U-shaped stirring frame 7 is arranged on the rotating shaft 6, and the U-shaped stirring frame 7 is attached to the bottom and the side wall of the hydrogenation chamber 1;
a second feeding pipe 9, an air inlet pipe 9' and an air return pipe 10 are arranged on the side wall of the hydrogenation bin 1;
the bottom of the hydrogenation bin 1 is connected with a filtering bin 14 through a liquid sending pipe 11, and the filtering bin 14 is connected with a crystallization bin 18 through a connecting pipe 17.
In the preferred scheme, hydrogenation storehouse 1 on still be equipped with baffle 3 on the position near the top, the equipartition is equipped with a plurality of unloading holes 301 on the baffle 3, is equipped with bearing 302 on the 3 central point of baffle position, pivot 6 passes bearing 302, is equipped with strip and the scraper blade 4 that is the level setting on the pivot 6 of baffle 3 top, the bottom surface and the 3 top surfaces contact of baffle of scraper blade 4.
In a preferable scheme, the number of the U-shaped stirring frames 7 is two, the two U-shaped stirring frames 7 are connected and fixed in a crossed manner, and the lower end of the rotating shaft 6 is fixedly arranged at the cross point of the two U-shaped stirring frames 7;
the rotating shaft 6 is provided with a vertical plate 8 which is positioned in the same vertical range with the vertical sections at the two sides of the U-shaped stirring frame 7.
In a preferred scheme, the air outlet end of the air inlet pipe 9' is arranged in the area between the vertical plate 8 and the vertical section of the U-shaped stirring frame 7.
In a preferable scheme, a slag tapping branch pipe 12 is arranged on the liquid conveying pipe 11.
In a preferable scheme, a negative pressure pump 15 is arranged on the filtering bin 14, and a water inlet pipe 16 is further arranged on the side wall of the filtering bin 14.
In a preferred embodiment, a first screen 171 is disposed in the connecting pipe 17.
In a preferable scheme, an acetone pipe 19 and an acetic acid pipe 21 are arranged on the side wall of the crystallization bin 18, a recovery pipe 20 is further arranged on the side wall of the crystallization bin 18 at a position close to the bottom, and a second filter screen 2001 is arranged in the recovery pipe 20;
the bottom of the crystallization bin 18 is provided with a discharge pipe 22.
Example 2:
the principle of the device is as follows:
a certain amount of methanol is fed into the hydrogenation chamber 1 through the second feeding pipe 9 in advance, then a condensate intermediate CBZ-L-valin-acyclovir produced after the esterification reaction is fed into the hydrogenation chamber 1 through the first feeding pipe 2, the condensate intermediate falls on the partition plate 3, at this time, the motor 5 is started, under the drive of the motor 5, the scraper 4 rotates and drives the condensate intermediate body falling on the partition plate 3 to rotate, due to the inclined arrangement of the scraper 4, the condensate intermediate is pressed and forced to fall through the blanking hole 301 into the methanol at the bottom of the hydrogenation chamber 1, meanwhile, the second feeding pipe 9 feeds the Pd/C catalyst into the hydrogenation chamber 1 and then feeds benzoic acid, hydrogen is introduced into the solution through the air inlet pipe 9' to carry out hydrogenation reaction, and the hydrogen continuously escapes in the whole process and is input through the air return pipe 10, so that the pressure in the hydrogenation bin 1 is always kept in a normal pressure state;
after the hydrogenation operation is completed, a valve on the liquid sending pipe 11 and the liquid sending pump 13 are opened, the solution which is filtered in the liquid sending pipe 11 enters the filtering bin 14, impurities are left on a filter screen in the liquid sending pipe 11 and can be discharged by opening the valve on the slag discharging branch pipe 12;
after a negative pressure pump 15 on the filtering bin 14 is started, vacuumizing and heating the filtering bin 14 to concentrate the solution, adding water into the filtering bin 14 through a water inlet pipe 16, and then opening a valve on a connecting pipe 17 to filter trace insoluble substances in the solution again;
and finally, the solution enters a crystallization bin 18, acetone is added into the solution again through an acetone pipe 19, at the moment, a solid is precipitated, a valve on a recovery pipe 20 is opened, crystals are filtered out through a second filter screen 2001, and then 95% acetic acid is introduced into the crystallization bin 18 through an acetic acid pipe 21 again for recrystallization, so that a valaciclovir product is finally obtained.
By adopting the structure, the utility model utilizes the structure that the baffle plate is matched with the scraper plate to ensure that the blanking points of the condensation compound intermediate of the solid are uniformly distributed in the hydrogenation bin, thereby ensuring the full mixing between the condensation compound intermediate and the methanol, shortening the time consumed by mixing and dissolving and improving the production efficiency; the driving of the scraping plate and the stirring frame is realized by using a single motor, so that the whole driving structure is simpler; the method realizes one-step operation in the whole hydrogenation reaction process, and other operations are not required to be carried out manually in the reaction process.
Claims (8)
1. Hydrochloric acid valaciclovir production is with hydrogenation reaction system, including hydrogenation storehouse (1), hydrogenation storehouse (1) top is equipped with first inlet pipe (2), characterized by: the top of the hydrogenation bin (1) is provided with a motor (5), the shaft of the motor (5) vertically penetrates downwards into the hydrogenation bin (1) and is connected with a rotating shaft (6) arranged in the hydrogenation bin (1) through a coupler, the rotating shaft (6) is provided with a U-shaped stirring frame (7), and the U-shaped stirring frame (7) is attached to the bottom and the side wall of the hydrogenation bin (1);
a second feeding pipe (9), an air inlet pipe (9') and an air return pipe (10) are arranged on the side wall of the hydrogenation bin (1);
the bottom of the hydrogenation bin (1) is connected with a filtering bin (14) through a liquid sending pipe (11), and the filtering bin (14) is connected with a crystallization bin (18) through a connecting pipe (17).
2. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 1, wherein: hydrogenation storehouse (1) on the inherent position that is close to the top still be equipped with baffle (3), the equipartition is equipped with a plurality of unloading holes (301) on baffle (3), be equipped with bearing (302) on baffle (3) central point position, bearing (302) are passed in pivot (6), be equipped with strip and be scraper blade (4) that the level set up on pivot (6) of baffle (3) top, the bottom surface and the contact of baffle (3) top surface of scraper blade (4).
3. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 1, wherein: the number of the U-shaped stirring frames (7) is two, the two U-shaped stirring frames (7) are connected and fixed in a cross manner, and the lower end of the rotating shaft (6) is fixedly arranged at the cross point of the two U-shaped stirring frames (7);
the rotating shaft (6) is provided with a vertical plate (8) which is positioned in the same vertical range with the vertical sections at the two sides of the U-shaped stirring frame (7).
4. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 3, wherein: the air outlet end of the air inlet pipe (9') is arranged in the area between the vertical plate (8) and the vertical section of the U-shaped stirring frame (7).
5. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 1, wherein: the liquid delivery pipe (11) is provided with a slag tapping branch pipe (12).
6. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 1, wherein: the filter bin (14) is provided with a negative pressure pump (15), and the side wall of the filter bin (14) is also provided with a water inlet pipe (16).
7. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 1, wherein: a first filter screen (171) is arranged in the connecting pipe (17).
8. The hydrogenation reaction system for valacyclovir hydrochloride production according to claim 1, wherein: an acetone pipe (19) and an acetic acid pipe (21) are arranged on the side wall of the crystallization bin (18), a recovery pipe (20) is further arranged on the side wall of the crystallization bin (18) at a position close to the bottom, and a second filter screen (2001) is arranged in the recovery pipe (20);
and a discharge pipe (22) is arranged at the bottom of the crystallization bin (18).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922367462.8U CN211570508U (en) | 2019-12-25 | 2019-12-25 | Hydrogenation reaction system for valaciclovir hydrochloride production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922367462.8U CN211570508U (en) | 2019-12-25 | 2019-12-25 | Hydrogenation reaction system for valaciclovir hydrochloride production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211570508U true CN211570508U (en) | 2020-09-25 |
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ID=72549294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201922367462.8U Active CN211570508U (en) | 2019-12-25 | 2019-12-25 | Hydrogenation reaction system for valaciclovir hydrochloride production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211570508U (en) |
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2019
- 2019-12-25 CN CN201922367462.8U patent/CN211570508U/en active Active
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