CN109762002A - A kind of cefathiamidine acetone water solvates monocrystalline and preparation method thereof - Google Patents
A kind of cefathiamidine acetone water solvates monocrystalline and preparation method thereof Download PDFInfo
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- CN109762002A CN109762002A CN201910089810.1A CN201910089810A CN109762002A CN 109762002 A CN109762002 A CN 109762002A CN 201910089810 A CN201910089810 A CN 201910089810A CN 109762002 A CN109762002 A CN 109762002A
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- cefathiamidine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/14—Compounds having a nitrogen atom directly attached in position 7
- C07D501/16—Compounds having a nitrogen atom directly attached in position 7 with a double bond between positions 2 and 3
- C07D501/20—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids
- C07D501/57—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids with a further substituent in position 7, e.g. cephamycines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/02—Preparation
- C07D501/04—Preparation from compounds already containing the ring or condensed ring systems, e.g. by dehydrogenation of the ring, by introduction, elimination or modification of substituents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Abstract
The invention discloses a kind of cefathiamidine acetone water solvates monocrystalline and preparation method thereof, which is colorless and transparent rhabdolith, belongs to rhombic system, space group P212121, cell parameter Unit cell volumeContain 2 molecule cefathiamidines, 3 molecule acetone and 2 molecular waters in each structure cell.In deionized water by the dissolution of cefathiamidine solid, the cefathiamidine solution of 0.05~2.00g/mL of mass concentration is prepared.Acetone is slowly added dropwise into the solution, acetone is made uniformly to spread over solution surface, is placed at 0 DEG C~25 DEG C and stands, obtains cefathiamidine acetone water solvates crystal.This method is easy to operate, can successfully prepare the crystal, and obtained monocrystalline pattern integrity degree is high.
Description
Technical field
The present invention relates to Cefathiamidine monocrystal and its preparation technical field more particularly to a kind of cefathiamidine acetone aqueous solvents
Compound monocrystalline and preparation method thereof.
Background technique
Cefathiamidine, chemical name (6R, 7R) -3- [(acetoxyl group) methyl] -7- [α-(N, N- diisopropylamidinateand sulfenyl)
Acetylamino] -8- oxo -5- thia -1- azabicyclo [4.2.0] oct-2-ene -2- formic acid betaine, white or off-white color knot
Crystalline substance powder, the molecular weight of anhydride are 472.57900, density 1.45g/cm.Due to its unique betaine structure, not
With being relatively easy to form solvate in solvent.Cefathiamidine belongs to first generation beta-lactam antibiotic, to gram positive bacteria, leather
Blue negative bacterium, Streptococcus viridans etc. have preferable antibacterial action.
Cefathiamidine has the unique molecular structure of amphoteric ion inner salt, and case of thermal instability is preparing cefathiamidine crystal
Process and its storage during, easily degrade, storage it is unstable；And hydrogen bond, product easily are formed with solvent in a solvent
Amorphous powder easy to form causes product purity bottom when precipitation, and quality does not meet medicinal standard；Therefore, to the development of its crystal form
The always hot spot of this field.
Cefathiamidine crystal form reported at present has: CN103556226A, CN1212324, CN100338072C are disclosed
Three kinds of cefathiamidine crystal forms, CN101074235B disclose a kind of cephalo-sulfide alcohol hydro-compound, CN102180890B,
CN104910186B discloses three kinds of cefathiamidine hydrates, and CN1898723 disclosed is a kind of unformed cefathiamidine.To mesh
It is preceding not there is patent disclosure to report cefathiamidine acetone water solvates monocrystalline yet.
Summary of the invention
The object of the present invention is to provide a kind of cefathiamidine acetone water solvates monocrystalline and preparation method thereof.
In a first aspect, a kind of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention, the monocrystalline are
Colorless and transparent rhabdolith belongs to rhombic system, space group P212121, cell parameter Unit cell volumeContain 2 molecule cephalos in each structure cell
Sulphur amidine, 3 molecule acetone and 2 molecular waters.
Preferably, the molecular formula of the monocrystalline: C47H78N8O17S4, molecular structural formula:
Second aspect, the embodiment of the invention also provides the preparation methods of above-mentioned cefathiamidine acetone water solvates monocrystalline
Are as follows:
Step 1: cefathiamidine solid and deionized water are configured to the cephalo sulphur that mass concentration is 0.05~2.00g/mL
Amidine solution；
Step 2: being slowly added dropwise acetone in Xiang Suoshu cefathiamidine solution, so that acetone uniformly spreads over the solution
Surface；
Step 3: surface is uniformly sprawled acetone cefathiamidine solution be placed on temperature be 0 DEG C~25 DEG C at stand 12~
48 hours, obtain cefathiamidine acetone water solvates monocrystalline.
Preferably, the mass concentration of cefathiamidine solution is 0.10~1.50g/mL in step 1.
Preferably, the quality for the acetone being added dropwise in step 2 be the cefathiamidine solution in deionized water quality 5~
25 times.
Preferably, the quality for the acetone being added dropwise in step 2 be the cefathiamidine solution in deionized water quality 10~
20 times.
Preferably, the time of repose in step 3 is 24 hours.
Preferably, the dwell temperature in step 3 is 5 DEG C~15 DEG C.
Preferably, the dwell temperature in step 3 is constant.
Cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention is a kind of from undisclosed of cefathiamidine
Novel crystal forms, and cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention have preferable stability.This
The preparation method for the cefathiamidine acetone water solvates monocrystalline that inventive embodiments provide, this method preparation can prepare cephalo sulphur
Amidine acetone water solvates monocrystalline, and crystalline product has the advantages that pattern integrity degree is high, crystallinity is high.And preparation manipulation letter
Single, equipment is simple.
It should be understood that above general description and following detailed description be only it is exemplary and explanatory, not
It can the limitation present invention.
Detailed description of the invention
In order to illustrate more clearly of technical solution of the present invention, letter will be made to attached drawing needed in the embodiment below
Singly introduce, it should be apparent that, for those of ordinary skills, without any creative labor,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is a kind of point of asymmetric cell of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention
Minor structure figure；
Fig. 2 is a kind of optical microscope of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention
Piece；
Fig. 3 is a kind of petrographic microscope figure of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention
Piece；
Fig. 4 is a kind of XRD spectrum of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention；
Fig. 5 is a kind of TG map of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention；
Fig. 6 is a kind of DSC map of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention
Fig. 7 is a kind of IR map of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention.
Specific embodiment
A kind of cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention, physicochemical properties are as follows:
(1) appearance is colorless and transparent rhabdolith；
(2) molecular formula: C47H78N8O17S4；
(3) molecular structural formula:
Cefathiamidine acetone water solvates single crystal data in the embodiment of the present invention is in German Brooker company Smart
It is acquired on 1000CCD single crystal diffractometer, using by graphite monochromatised Cu K alpha ray (λ=0.154184nm).Minimum deflection
Factor R1=0.0381, wR2=0.1039.Crystal belongs to rhombic system, space group P212121, cell parameter C=25.3588 (2), unit cell volumeEach structure cell
In contain 2 molecule cefathiamidines, 3 molecule acetone and 2 molecular waters.Relative molecular mass is 1155.41, density 1.244g/
cm3.Its molecular structure is as shown in Figure 1.
The embodiment of the invention also provides the preparation methods of above-mentioned cefathiamidine acetone water solvates monocrystalline.
Step 1: cefathiamidine solid and deionized water are configured to the cephalo sulphur that mass concentration is 0.05~2.00g/mL
Amidine solution.
In the specific implementation process, the mass concentration preferred scope of the cefathiamidine solution of configuration is 0.10~1.50g/
mL。
Step 2: being slowly added dropwise acetone in Xiang Suoshu cefathiamidine solution, so that acetone uniformly spreads over the solution
Surface.
In the specific implementation process, the quality of the acetone of dropwise addition is deionized water in the cefathiamidine solution in step 1
5~25 times of amount.
In a kind of possible embodiment, the preferred scope of the quality of the acetone of dropwise addition is that cefathiamidine is molten in step 1
10~20 times of deionized water quality in liquid.
Step 3: surface is uniformly sprawled acetone cefathiamidine solution be placed on temperature be 0 DEG C~25 DEG C at stand 12~
48 hours, obtain cefathiamidine acetone water solvates monocrystalline.
In a kind of possible embodiment, the cefathiamidine solution that acetone is uniformly sprawled on surface is placed on quiet at 0 DEG C~25 DEG C
It sets 24 hours, begins within about 12 hours crystallite generation, subsequent crystal is slowly grown, and cefathiamidine acetone aqueous solvent can be obtained
Object monocrystalline.In the specific implementation process, it is 5 DEG C that the dwell temperature preferred scope of the cefathiamidine solution of acetone is uniformly sprawled on surface
~15 DEG C.In a kind of possible embodiment, the dwell temperature that the cefathiamidine solution of acetone is uniformly sprawled on surface is constant,
In specific implementation process, it is believed that temperature is constant at a set temperature in set temperature ± 2 DEG C.
The obtained crystal of this method is rhabdolith, as shown in Figure 2；With polarized light property and crystallinity height, such as Fig. 3 institute
Show；The diffracted intensity higher peak position of XRD be 2 θ=7.846 °, 10.402 °, 12.143 °, 15.706 °, as shown in Figure 4；Product
There is weightlessness before 373K, represent the removing of acetone solvent, the weightlessness between 373K~393K has corresponded to the de- of hydrone
It removes, as shown in Figure 5；And need to absorb heat when losing acetone and water, when cefathiamidine molecular scission can heat release, as shown in Figure 6；It is infrared
Spectrum is as shown in Figure 7.This method preparation can prepare cefathiamidine acetone water solvates monocrystalline, and crystalline product has pattern
The advantage that integrity degree is high, crystallinity is high.
Embodiment 1
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 0.05g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle, the purpose for crossing 0.22 μm of water system filter membrane is to filter the solution.By 15 times of deionized water quality used
Acetone slowly spreads in cefathiamidine solution surface by dropper, will be statically placed in 15 DEG C of insulating boxs after serum bottle closure, 24 is small
When after by crystal taking-up analyzed and characterized.Using German 1000 CCD single crystal diffractometer of Brooker company Smart, to institute
It obtains crystal prototype to be analyzed, the results are shown in Table 1~6 and attached drawing 1~7.
Table 1 is crystal data and structure optimization data；
Table 2 is non-hydrogen atom coordinate
Table 3 is bond distance
Table 4 is bond angle (°)；
Table 5 is hydrogen atom coordinates
Table 6 is the peak position XRD coordinate.
Crystal be it is colorless and transparent rodlike, using German 1000 CCD single crystal diffractometer of Brooker company Smart, use warp
Graphite monochromatised Cu K alpha ray (λ=0.154184nm) is crossed to be analyzed.Minimum deflection factor R1=0.0381, wR2=
0.1039.The crystal is monocrystalline, belongs to rhombic system, space group P212121, cell parameter C=25.3588 (2), unit cell volumeContain 2 molecule cephalos in each structure cell
Sulphur amidine, 3 molecule acetone and 2 molecular waters.Relative molecular mass is 1155.41, density 1.244g/cm3.Specific data and fitting
Structure cell figure is shown in Table 1~6 and attached drawing 1~7.
Embodiment 2
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 0.10g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 3
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.00g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 4
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 5
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 2.00g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 6
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.5 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper, it will
It is statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up is analyzed and characterized after 24 hours.To gained crystalloids
Product are analyzed, the results showed that gained crystal is identical as the cefathiamidine acetone water solvates mono-crystalline type in embodiment 1.
Embodiment 7
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.10 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 8
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.20 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 9
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.25 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 15 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 10
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 0 DEG C of insulating box, crystal taking-up analyzed and characterized after 24 hours.To gained crystalloids
Product are analyzed, the results showed that gained crystal is identical as the cefathiamidine acetone water solvates mono-crystalline type in embodiment 1.
Embodiment 11
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 5 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystalloids
Product are analyzed, the results showed that gained crystal is identical as the cefathiamidine acetone water solvates mono-crystalline type in embodiment 1.
Embodiment 12
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 10 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
Embodiment 13
In clean beaker intermediate ion water and high-purity cefathiamidine anhydride solid, preparing cefathiamidine mass concentration is
The solution of 1.50g/mL, solution are put into stirring and dissolving in ultrasonic tank, after the water system filter membrane for taking the solution to cross 0.22 μm with syringe
It injects in serum bottle.15 times of deionized water quality of acetone used is slowly spread in into cefathiamidine solution surface by dropper,
It will be statically placed in after serum bottle closure in 25 DEG C of insulating boxs, crystal taking-up analyzed and characterized after 24 hours.To gained crystal
Sample is analyzed, the results showed that gained crystal and the cefathiamidine acetone water solvates mono-crystalline type phase in embodiment 1
Together.
1 crystal data of table and structure optimization data
2 non-hydrogen atom coordinate of table
3 bond distance of table
4 bond angle (°) of table
5 hydrogen atom coordinates of table
6 peak position XRD coordinate of table
Cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention is a kind of from undisclosed of cefathiamidine
Novel crystal forms, and cefathiamidine acetone water solvates monocrystalline provided in an embodiment of the present invention have preferable stability.This
The preparation method for the cefathiamidine acetone water solvates monocrystalline that inventive embodiments provide, this method preparation can prepare cephalo sulphur
Amidine acetone water solvates monocrystalline, and crystalline product has the advantages that pattern integrity degree is high, crystallinity is high.And preparation manipulation letter
Single, equipment is simple.
Same and similar part may refer to each other between each embodiment in this specification.
Those skilled in the art will readily occur to of the invention its after considering specification and the disclosure invented here of practice
Its embodiment.This application is intended to cover any variations, uses, or adaptations of the invention, these modifications, purposes or
Person's adaptive change follows general principle of the invention and including the undocumented common knowledge in the art of the present invention
Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following
Claim is pointed out.
Invention described above embodiment is not intended to limit the scope of the present invention..
Claims (9)
1. a kind of cefathiamidine acetone water solvates monocrystalline, which is characterized in that
The monocrystalline is colorless and transparent rhabdolith, belongs to rhombic system, space group P212121, cell parameterUnit cell volumeEach crystalline substance
Contain 2 molecule cefathiamidines, 3 molecule acetone and 2 molecular waters in born of the same parents.
2. cefathiamidine acetone water solvates monocrystalline as described in claim 1, which is characterized in that the molecule of the monocrystalline
Formula: C47H78N8O17S4, molecular structural formula:
3. a kind of preparation method of cefathiamidine acetone water solvates monocrystalline, which is characterized in that
Step 1: it is molten that cefathiamidine solid and deionized water are configured to the cefathiamidine that mass concentration is 0.05~2.00g/mL
Liquid；
Step 2: being slowly added dropwise acetone in Xiang Suoshu cefathiamidine solution, so that acetone uniformly spreads over the surface of the solution；
Step 3: it is that standing 12~48 is small at 0 DEG C~25 DEG C that the cefathiamidine solution that surface is uniformly sprawled to acetone, which is placed on temperature,
When, obtain cefathiamidine acetone water solvates monocrystalline.
4. preparation method as claimed in claim 3, which is characterized in that the mass concentration of cefathiamidine solution is in step 1
0.10~1.50g/mL.
5. preparation method as claimed in claim 3, which is characterized in that the quality for the acetone being added dropwise in step 2 is the cephalo
5~25 times of deionized water quality in sulphur amidine solution.
6. preparation method as claimed in claim 5, which is characterized in that the quality for the acetone being added dropwise in step 2 is the cephalo
10~20 times of deionized water quality in sulphur amidine solution.
7. preparation method as claimed in claim 3, which is characterized in that the time of repose in step 3 is 24 hours.
8. preparation method as claimed in claim 3, which is characterized in that the dwell temperature in step 3 is 5 DEG C~15 DEG C.
9. preparation method as claimed in claim 3, which is characterized in that the dwell temperature in step 3 is constant.
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| CN101074235A (en) * | 2006-05-15 | 2007-11-21 | 中国药品生物制品检定所 | Cephalo-sulfide alcohol hydro-compound and its production |
| CN104530082A (en) * | 2014-12-08 | 2015-04-22 | 悦康药业集团有限公司 | Cefathiamidine compound |
| CN104910186A (en) * | 2015-05-12 | 2015-09-16 | 山东罗欣药业集团股份有限公司 | Cefathiamidine compound |
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| CN101074235A (en) * | 2006-05-15 | 2007-11-21 | 中国药品生物制品检定所 | Cephalo-sulfide alcohol hydro-compound and its production |
| CN104530082A (en) * | 2014-12-08 | 2015-04-22 | 悦康药业集团有限公司 | Cefathiamidine compound |
| CN104910186A (en) * | 2015-05-12 | 2015-09-16 | 山东罗欣药业集团股份有限公司 | Cefathiamidine compound |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111018890A (en) * | 2019-01-30 | 2020-04-17 | 山东省分析测试中心 | Cefathiamidine acetone hydrosolvent single crystal and preparation method thereof |
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