CN206152402U - Thio iminazole quinoline ketone compound's chromatography column - Google Patents
Thio iminazole quinoline ketone compound's chromatography column Download PDFInfo
- Publication number
- CN206152402U CN206152402U CN201621163820.3U CN201621163820U CN206152402U CN 206152402 U CN206152402 U CN 206152402U CN 201621163820 U CN201621163820 U CN 201621163820U CN 206152402 U CN206152402 U CN 206152402U
- Authority
- CN
- China
- Prior art keywords
- chromatographic column
- main body
- column main
- thioic
- chromatography column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- -1 Thio iminazole quinoline ketone compound Chemical class 0.000 title claims abstract description 27
- 238000004587 chromatography analysis Methods 0.000 title abstract description 20
- SMWDFEZZVXVKRB-UHFFFAOYSA-N anhydrous quinoline Natural products N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 title abstract 2
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000003480 eluent Substances 0.000 claims description 17
- 239000000945 filler Substances 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- 238000002955 isolation Methods 0.000 claims description 10
- 239000010410 layer Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011229 interlayer Substances 0.000 claims description 7
- 230000007246 mechanism Effects 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 239000005336 safety glass Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract 1
- 238000004440 column chromatography Methods 0.000 description 6
- 238000010828 elution Methods 0.000 description 6
- 150000001263 acyl chlorides Chemical class 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- CAAMSDWKXXPUJR-UHFFFAOYSA-N 3,5-dihydro-4H-imidazol-4-one Chemical class O=C1CNC=N1 CAAMSDWKXXPUJR-UHFFFAOYSA-N 0.000 description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001953 recrystallisation Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 150000002540 isothiocyanates Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- WQJONRMBVKFKOB-UHFFFAOYSA-N cyanatosulfanyl cyanate Chemical compound N#COSOC#N WQJONRMBVKFKOB-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 238000009333 weeding Methods 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The utility model provides a thio iminazole quinoline ketone compound's chromatography column, its has the chromatography column main part, its top -down of divide into two sections, connect through cup jointing locking device between two sections, the upper end of chromatography column main part has been installed and has been covered the structure, and the top of chromatography column main part is provided with eluate storage device and washing liquid storage device, the surface of chromatography column main part closely wraps up there is column temperature management device, closely wrap up the outside of column temperature management device has the isolated cover that keeps warm, chromatography column main part below is equipped with receiving arrangement, and during receiving arrangement's upper end was inserted to the lower part of chromatography column main part, the evacuation pump was connected by the vacuum connecting pipe to the lateral wall of this receiving arrangement's upper end. The utility model discloses production equipment operation is convenient, system simple structure, low in manufacturing cost.
Description
Technical field
The utility model is related to chromatography field, and in particular to a kind of chromatographic column of thioic imidazolone compound.
Background technology
Many imidazolone compounds have good activity of weeding, and environment compatibility is good, hold in nature
It is degradable.Although having carried out to imidazolone compound structural modification in prior art, the functional group for introducing is mostly
Imines, ureas etc., introducing amide-type active function groups are little to the report that imidazolone carries out structural modification.
The raw material isothiocyanates and initiation material aniline of new imidazolone compound is all liquid, and different sulphur
Cyanate Nature comparison is active and boiling point is higher, and the way of distillation is difficult to the sterling that obtains in high yield, therefore using column chromatography pair
It is separated；The polarity of intermediate substituted imidazolinones is larger, most of raw material reaction completely, intermediate and acyl chloride reaction
Target compound is generated, accessory substance is less, reaction relatively fully, can obtain sterling through recrystallization in theory；But pass through
Experiment finds that acyl chlorides is very active, inevitably hydrolyzes during the course of the reaction, causes the presence of acid in reaction system,
Recrystallization is not easy to remove.The purifying of object need to take the means of column chromatography.
Chromatographic column is very universal as the common equipment application for isolating and purifying, and in prior art, chromatographic column mostly is straight tube post
Shape structure, when elution is used, especially the chromatographic column of dry column-packing, due to mechanics effect, connects with chromatographic column inner surface
Tactile partial filler always infiltrates prior to middle filler, causes the distortion of column chromatography band to broaden, and reduces separating degree.As
The background technology of the application, patent document 1 (CN203389364U) discloses a kind of chromatographic column, and the chromatographic column includes at least two
Individual different solid layer, by taking double-deck chromatographic column as an example, is made up of, described first the first solid layer and the second solid layer series coupled
Solid layer is made up of anion-exchange membrane or microballon, and second solid layer is made up of pellosil or microballon, the chromatography
Rod structure is simple, easy to use.Patent document 2 (CN201115795Y) discloses a kind of Novel chromatographic column, and it includes cylinder, post
The connector of body upper end is standard frosted mouth, and in the bottom of cylinder the minim pipette of integrally connected is provided with, and is set in minim pipette
There is teflon piston.The utility model connects when using with liquid feeding ball or pressue device, and sealing is preferable, will not produce Lou
The phenomenon of liquid.Additionally, can be closely coupled with liquid feeding ball or pressue device by barb with the thing such as rope or rubber band, therefore cylinder
The stronger pressure that inside can bear so that solution can be separated out in the presence of suppressing by thin layer silica gel, and elute consuming
Time is shorter and final effect is also preferable.
However, the device that patent document 1 and 2 is adopted there are problems that a series of, for example elution efficiency is low, causes
A large amount of wastes of eluant, eluent, the yield of sample is low, and the high expensive of chromatography.
Background technology document：
Patent document 1：CN203389364U, patent document 2：CN201115795Y.
Utility model content
1. the technical problem to be solved
Based on the above-mentioned problems in the prior art, the purpose of this utility model is to provide a kind of thiocarbamoyl imidazole quinoline ketone
The chromatographic column of class compound.
2. technical scheme
The purpose of this utility model is mainly realized by following technical scheme.
A kind of chromatographic column of thioic imidazolone compound, it has chromatographic column main body, and it is divided into from top to bottom two sections,
By socket locking device connection between described two sections, the upper end of chromatographic column main body is equiped with lid structure, chromatographic column main body it is upper
Side is provided with eluent receptacle and cleaning solution receptacle, and the eluent receptacle and cleaning solution receptacle are respectively by penetrating
The connecting tube of lid structure is connected with chromatographic column main body；The outer surface tight of the chromatographic column main body has column temperature managing device,
The outside tight of the column temperature managing device has insulation isolation set, and the bore of chromatographic column main body bottom reduces and be provided with cut-off
Mechanism；Chromatographic column main body lower section is provided with reception device, in the upper end of the bottom insertion reception device of chromatographic column main body, the reception dress
The side wall of the upper end put connects vacuum pumping pump by vacuum connection tube.
Preferably, device for converting electric energy is provided with the outer surface of insulation isolation set, the disabling mechanism is flow-stop valve.
Preferably, the bottom of the reception device is provided with interlayer, and liquid nitrogen is provided with interlayer.
Preferably, the chromatographic column main body, eluent receptacle and cleaning solution receptacle pass through respectively connection mounting structure
Connection is on the support frame.
Preferably, filler protection device is provided with the top of the chromatographic column main body, it is three helical layer structures, the spiral
Structure is curved form.
Preferably, electrical energy conversion circuit is provided with the device for converting electric energy, in the connecting tube valve is provided with.
Preferably, resistance wire is provided with the column temperature managing device, the temperature of resistance wire is controlled by controller, and arranged
There is temperature indicating device.
Preferably, the material of the insulation isolation set is to receive the heat-insulated soft felt of base.
Preferably, the agent structure of the chromatographic column main body is safety glass, and the eluant, eluent solvent that the chromatographic column is used is
The intermixture of ethyl acetate and petroleum ether.
3. beneficial effect
Compared with prior art, the beneficial effect of the chromatographic column of thioic imidazolone compound of the present utility model exists
In：
The utility model equipment can be taken out reception device and chromatographic column main body lower space for negative pressure by vavuum pump, from
And the reagent flow rate in chromatographic column is improved, save disengaging time.
The utility model equipment adopts said structure design, and its lamps structure is simple, easy to operate advantage, and filler used
Reuse after cleaning, improve filler utilization rate, reduce chromatography cost.
The utility model in use can be with sample in elution post, while also can be by two-stage chromatography column main body
In filler take out, individually wash-out, so that elution efficiency is improved, saves eluting agent, and improves the yield of sample；Together
When controllable chromatographic column temperature, the controllability of temperature is strong, be easy to according to different biological chromatographies need adjust temperature, system knot
Structure is simple, low cost of manufacture.
Description of the drawings
Fig. 1 is a kind of chromatographic column of the thioic imidazolone compound constituted according to the utility model preferred embodiment
Schematic diagram.
In figure：
1- chromatographic column main bodies；2- insulation isolation sets；3- device for converting electric energy；4- column temperature managing devices；5- support frames；6-
Lid structure；7- connecting tubes；8- eluent receptacles；9- cleaning solution receptacles；10- disabling mechanisms；11- vacuum connection tubes；12- connects
Receiving apparatus；13- vacuum pumping pumps；14- interlayers.
Specific embodiment
Hereinafter, refer to the attached drawing is described in detail to specific embodiment of the utility model, it is detailed according to these
Thin description, one of ordinary skill in the art can implement the utility model it can be clearly understood that the utility model.Do not disobeying
In the case of back of the body the utility model principle, the feature in each different embodiment can be combined to obtain new embodiment party
Formula, or some of some embodiments feature is substituted, obtain other and preferably implement embodiment.
As shown in figure 1, a kind of chromatographic column of thioic imidazolone compound, it has chromatographic column main body 1, its from upper and
Under be divided into two sections, between described two sections by socket locking device connection, can be by two-stage chromatography column main body 1 after being used for multiple times
Filler takes out, individually wash-out.The upper end of chromatographic column main body 1 is equiped with lid structure 6, and the top of chromatographic column main body 1 is provided with wash-out
Liquid receptacle 8 and cleaning solution receptacle 9, the eluent receptacle 8 and cleaning solution receptacle 9 are respectively by penetrating lid structure 6
Connecting tube 7 connect with chromatographic column main body 1；Chromatography is carried out by the eluent of installing in eluent receptacle 8, knot is separated
After beam filler is cleaned by the cleaning fluid in cleaning solution receptacle 9, reused after filler cleaning used.The chromatography
The outside tight that the outer surface tight of post main body 1 has column temperature managing device 4, the column temperature managing device 4 has insulation
Isolation set 2, the bore of the bottom of chromatographic column main body 1 reduces and is provided with disabling mechanism 10；The lower section of chromatographic column main body 1 is provided with reception device
12, in the upper end of the bottom insertion reception device 12 of chromatographic column main body 1, the side wall of the upper end of the reception device 12 is by bonding in vacuum
Pipe 11 connects vacuum pumping pump 13.
Device for converting electric energy 3 is provided with the outer surface of insulation isolation set 2, the disabling mechanism 10 is flow-stop valve.
The bottom of the reception device 12 is provided with interlayer 14, and liquid nitrogen is provided with interlayer.During vacuumizing, device
Interior product can produce volatilization, using the product of the recyclable volatilization of liquid nitrogen, reduce waste.
The chromatographic column main body 1, eluent receptacle 8 and cleaning solution receptacle 9 are connected respectively by connection mounting structure
In support frame 5.
Filler protection device is provided with the top of the chromatographic column main body 1, it is three helical layer structures, the helical structure is
Curved form.Such structure can slow down eluant, eluent into the flow velocity of chromatographic column, prevent from making the crossing large impact of filler in post
The destruction of filler in pairs.
Electrical energy conversion circuit is provided with the device for converting electric energy 3, direct current can be converted to certain frequency
Alternating current, excited oscillation is produced with this to chromatographic column, the filler being capable of achieving in quick consolidation post.Chromatographic column main body 1 is propped up with being connected
The connection tightness of frame structure meets the excited oscillation.Valve is provided with the connecting tube 7.
Resistance wire is provided with the column temperature managing device 4, the temperature of resistance wire is controlled by controller, and be provided with temperature
Display device, such setting can ensure the reaction temperature in post, be further ensured that reaction effect so as to being optimal
As a result.
The material of the insulation isolation set 2 is further ensured that reaction temperature to receive the heat-insulated soft felt of base, prevents temperature change pair
The impact that reaction is caused.
The agent structure of the chromatographic column main body 1 is safety glass, and the eluant, eluent solvent that the chromatographic column is used is acetic acid second
The intermixture of ester and petroleum ether.
The synthesis of thioic imidazolone compound prepares isothiocyanates by initiation material of amine, then with substituted-amino
Acid reaction obtains the key intermediate containing imidazolone ring, and intermediate obtains final product with acyl chloride reaction.Raw material isothiocyanic acid
Ester and initiation material aniline are all liquid, and isothiocyanates Nature comparison is active and boiling point is higher, and the way of distillation is difficult to height
Yield obtains sterling, therefore it is separated using column chromatography；It is final to choose ethyl acetate and petroleum ether mixture
Used as column chromatography solvent, thiocarbamoyl imidazole quinoline ketone yield is more than 79% for system；Intermediate generates target compound with acyl chloride reaction, secondary
Product is less, and reaction relatively fully, can obtain sterling through recrystallization in theory；But pass through experiment and find that acyl chlorides is very
Vivaciously, inevitably hydrolyze during the course of the reaction, cause the presence of acid in reaction system, recrystallization to be not easy to remove.
The purifying of object takes the means of column chromatography, using ethyl acetate and petroleum ether mixed solvent as eluant, eluent, purification
Target product yield is more than 75%.
The utility model equipment can be taken out reception device and chromatographic column main body lower space for negative pressure by vavuum pump, from
And the reagent flow rate in chromatographic column is improved, save disengaging time.Additionally, using said structure design, its lamps structure is simple, operation
Reuse after convenient advantage, and filler used cleaning, improve filler utilization rate, reduce chromatography cost.This reality
Sample in elution post can be used in use with new, while can also take the filler in two-stage chromatography column main body
Go out, individually wash-out, so that elution efficiency is improved, save eluting agent, and improve the yield of sample；While controllable preparative layer
The temperature of post is analysed, the controllability of temperature is strong, be easy to need regulation temperature according to different biological chromatographies, system architecture is simple, system
Make low cost.
Although being described to the utility model above by referring to specific embodiment, art technology people
Member for the utility model is disclosed it should be appreciated that in the utility model principle disclosed and scope, can configure and details
Make many modifications.Protection domain of the present utility model is determined by appended claim, and claim is intended to
Whole modifications that the equivalent literal meaning or scope of technical characteristic is included in claim.
Claims (9)
1. a kind of chromatographic column of thioic imidazolone compound, it is characterised in that with chromatographic column main body (1), its from upper and
Under be divided into two sections, between described two sections by socket locking device connection, the upper end of chromatographic column main body (1) is equiped with lid structure
(6) eluent receptacle (8) and cleaning solution receptacle (9), the eluent storage, are provided with above chromatographic column main body (1)
Device (8) and cleaning solution receptacle (9) are connected respectively by penetrating the connecting tube (7) of lid structure (6) with chromatographic column main body (1)；Institute
Stating the outer surface tight of chromatographic column main body (1) has column temperature managing device (4), and the outside of the column temperature managing device (4) is tight
Close to be enclosed with insulation isolation set (2), the bore of chromatographic column main body (1) bottom reduces and is provided with disabling mechanism (10)；Chromatographic column master
Body (1) lower section is provided with reception device (12), in the upper end of bottom insertion reception device (12) of chromatographic column main body (1), the reception
The side wall of the upper end of device (12) is by vacuum connection tube (11) connection vacuum pumping pump (13).
2. the chromatographic column of thioic imidazolone compound as claimed in claim 1, it is characterised in that insulation isolation set (2)
Outer surface on be provided with device for converting electric energy (3), the disabling mechanism (10) is flow-stop valve.
3. the chromatographic column of thioic imidazolone compound as claimed in claim 2, it is characterised in that the reception device
(12) bottom is provided with interlayer (14), and liquid nitrogen is provided with interlayer.
4. the chromatographic column of thioic imidazolone compound as claimed in claim 3, it is characterised in that the chromatographic column main body
(1), eluent receptacle (8) and cleaning solution receptacle (9) are connected in support frame (5) respectively by connection mounting structure.
5. the chromatographic column of thioic imidazolone compound as claimed in claim 4, it is characterised in that the chromatographic column main body
(1) filler protection device is provided with top, it is three helical layer structures, the helical structure is curved form.
6. the chromatographic column of thioic imidazolone compound as claimed in claim 5, it is characterised in that the electric energy converting means
Put and be provided with (3) electrical energy conversion circuit, on the connecting tube (7) valve is provided with.
7. the chromatographic column of thioic imidazolone compound as claimed in claim 6, it is characterised in that the column temperature management dress
Put in (4) and be provided with resistance wire, the temperature of resistance wire is controlled by controller, and be provided with temperature indicating device.
8. the chromatographic column of thioic imidazolone compound as claimed in claim 7, it is characterised in that the insulation isolation set
(2) material is to receive the heat-insulated soft felt of base.
9. the chromatographic column of thioic imidazolone compound as claimed in claim 8, it is characterised in that the chromatographic column main body
(1) agent structure is safety glass, and the eluant, eluent solvent that the chromatographic column is used is the intermixture of ethyl acetate and petroleum ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621163820.3U CN206152402U (en) | 2016-10-25 | 2016-10-25 | Thio iminazole quinoline ketone compound's chromatography column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621163820.3U CN206152402U (en) | 2016-10-25 | 2016-10-25 | Thio iminazole quinoline ketone compound's chromatography column |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206152402U true CN206152402U (en) | 2017-05-10 |
Family
ID=58656305
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201621163820.3U Expired - Fee Related CN206152402U (en) | 2016-10-25 | 2016-10-25 | Thio iminazole quinoline ketone compound's chromatography column |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206152402U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107261559A (en) * | 2017-07-13 | 2017-10-20 | 江苏联宇医疗器械有限公司 | A kind of pharmaceutical chromatographic column |
| CN111729351A (en) * | 2020-07-29 | 2020-10-02 | 辽宁石化职业技术学院 | Novel automatic chromatographic separation purification device |
-
2016
- 2016-10-25 CN CN201621163820.3U patent/CN206152402U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107261559A (en) * | 2017-07-13 | 2017-10-20 | 江苏联宇医疗器械有限公司 | A kind of pharmaceutical chromatographic column |
| CN111729351A (en) * | 2020-07-29 | 2020-10-02 | 辽宁石化职业技术学院 | Novel automatic chromatographic separation purification device |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
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| CF01 | Termination of patent right due to non-payment of annual fee |