Crystallization method of cefcapene ester hydrochloride monohydrate
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A technology for cefcapine hydrochloride and monohydrate, which is applied in the field of crystallization of cefcapine hydrochloride monohydrate, and achieves the effects of being beneficial to drying, beneficial to solvent recovery and good clarity
Active Publication Date: 2010-10-20
FUJIAN FUKANG PHARMA
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[0005] Due to the poor stability of cefcapene pivoxil hydrochloride, its 7-position amide side chain, 3-position carboxamide, and 4-position pivaloyloxymethyl ester Cefcapene axetil hydrochloride under the conditions of long time, high temperature, over-acid and over-alkali will degrade to varying degrees, resulting in darker color and lower content
Cefcapene pivoxil hydrochloride is converted into cefcapene pivoxil hydrochloride monohydrate process. Due to factors such as solvent type, concentration and dosage of hydrochloric acid, water volume, drop rate, temperature, etc., the yield of cefcapene pivoxil hydrochloride monohydrate crystals is low, and the quality Poor, for example, if the temperature is too high and the acidity is too strong, the impurities in the finished product will be large. When the amount of alcohol in the crystallization system increases, the crystallization process will be difficult to control; The particle size, looseness, crushing difficulty, and solubility are all different, which have a certain impact on the quality of the finished product
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Embodiment 1
[0027] 1. Cool 5ml of methanol to below 10°C (-5°C to 10°C), and add 1g of cefcapene hydrochloride to dissolve it.
[0028] 3. Add 0.05g of activated carbon to decarbonize for 20-30 minutes, filter, and wash with a small amount of methanol solution; the obtained solution is solution 1.
[0029] 4. Put 7ml of deionized water and 0.5ml of 30% hydrochloric acid into another reaction kettle and mix. The solution is solution 2, and the temperature is controlled at 20-30°C.
[0030] 6. Add solution 1 dropwise to solution 2 to crystallize (you can also add solution 2 to solution 1 to crystallize). During the dropping process, ensure that the temperature of solution 1 is below 10°C (-5 to 10°C).
[0031] 7. After the dropwise addition, keep stirring at the above temperature for 1 hour, and then cool the temperature to below 10°C.
[0032] 8. Stir at the same temperature (below 10°C) for 1 hour and filter the resulting crystals.
[0033] 9. The crystallization filter cake was washed ...
Embodiment 2
[0036] 1. Cool the mixture of 50ml of methanol and 50ml of acetone to below 10°C (-5°C to 10°C), and add 10g of cefcapene hydrochloride to dissolve it.
[0037] 3. Add 1g of activated carbon to decarbonize for 20-30 minutes, filter, and wash with a small amount of methanol solution; the obtained solution is solution 1.
[0038] 4. Put 80ml of deionized water and 10ml of 36% hydrochloric acid into another reaction kettle to mix. The solution is solution 2, and the temperature is controlled at 5-20°C.
[0039] 6. Add solution 1 dropwise to solution 2 to crystallize (you can also add solution 2 to solution 1 to crystallize). During the dropping process, ensure that the temperature of solution 1 is below 10°C (-5 to 10°C).
[0040] 7. After the dropwise addition, keep stirring at the above temperature for 2 hours, and then cool the temperature to below 10°C.
[0041] 8. Stir at the same temperature (below 10°C) for 2 hours and then filter the resulting crystals.
[0042] 9. The ...
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Abstract
The invention relates to a crystallization method of cefcapene ester hydrochloride monohydrate, which belongs to the field of medicine. The method comprises the following steps: adding solvents into cefcapene ester hydrochloride for dissolution; adding active carbon for decolourization; carrying out filtration and washing; adding hydrochloric acid water solution into obtained filter liquid for carrying out crystallization; filtering crystals; respectively washing the crystals by water and ethyl acetate; and carrying out drying to obtain the cefcapene ester hydrochloride monohydrate. The method of the invention can use a single solvent of methanol for crystallization to improve the recovery yield and reduce the production cost, and can also use mixed solvents of the methanol and ketone for crystallization to improve the quality of finished product. Low-temperature active carbon is used for decolourization, and the impurity control in the operation process can be ensured at the same time of ensuring the product quality (the control on the color grade, the endotoxin and the like). The baking temperature is reduced, the baking time is shortened, and the quality such as the color grade, the impurity content and the like of the products can be reached. The invention has the advantages of simplicity, easy implementation, low cost, good crystallization clarity, good color grade and easy control on the impurities of the finished products, is suitable for large-scale popularized application, and has obvious economic benefits.
Description
technical field [0001] The invention relates to a crystallization method of cefcapene hydrochloride monohydrate, which belongs to the field of medicines. Background technique [0002] Cefcapene pivoxil hydrochloride is the third generation of oral cephalosporin antibiotics, used for the treatment of superficial infection caused by sensitive bacteria, deep skin infection, chronic pyoderma, secondary infection of wounds such as trauma, burns and surgical trauma, mastitis , perianal abscess, pharyngitis, laryngitis, tonsillitis (including peritonsillar inflammation, peritonsillar abscess), acute bronchitis, pneumonia, secondary infection of chronic respiratory diseases, cystitis, pyelonephritis, urethritis, cervicitis , cholecystitis, cholangitis, intrauterine infection, uterine adnexitis, dacryocystitis, stye, meibomitis, otitis externa, otitis media, sinusitis, dental tissue infection, periodontitis, jaw inflammation, etc. Cefcapene pivoxil hydrochloride is an ester-type p...
Claims
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Application Information
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