Cefradine compound containing half water

A cefradine and compound technology, which is applied in the field of 1/2 water cefradine compound and its preparation, can solve the problems of backward preparation method, instability between batches and high impurities

Inactive Publication Date: 2019-01-04
陕西顿斯制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, compared with similar foreign products, domestic cephradine has problems such as uneven particle size distribution, poor fluidity, high impurities, and poor stability.
These problems are mainly caused by backward preparation methods.
The existence of these problems leads to poor product quality and instability between batches on the one hand, and also leads to increased production costs and waste of raw materials to a certain extent.

Method used

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  • Cefradine compound containing half water
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  • Cefradine compound containing half water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the preparation of 1 / 2 water cephradine compound

[0033] Dissolve 10.1 g of crude cephradine in 100.4 g of water, control the temperature in a water bath at 35 ° C, add 0.5 g of activated carbon, stir and absorb for 30 min, and filter; adjust the pH value of the filtrate to 6.0 with hydrochloric acid; slowly add the dissolving agent dichloride to the above solution Methane, filter, wash the filter cake with ethanol 30mL×2; dissolve the filter cake in a mixed solution of 700mL water and methanol (6:1), stir to dissolve; add seed crystals, control the temperature at 8°C, and stand for crystallization for 3h , filtered; the filtrate was washed with 30 mL of ethanol × 2, and dried in vacuum at 25° C. for 40 min to obtain 9.78 g of 1 / 2 water cephradine compound.

[0034] The X-ray powder diffraction pattern has characteristic diffraction peaks at diffraction angles 2θ of 7.25°, 10.98°, 14.53°, 16.28°, 17.80°, 19.38°, 20.21°, 22.06°, and 22.90°. The relative di...

Embodiment 2

[0037] Embodiment 2: the preparation of 1 / 2 water cephradine compound

[0038] Dissolve 15.3 g of crude cephradine in 150.1 g of water, control the temperature in a water bath at 30 ° C, add 0.7 g of activated carbon, stir and adsorb for 30 min, and filter; adjust the pH value of the filtrate to 6.5 with hydrochloric acid; slowly add the dissolution agent trichloride to the above solution Methane, filter, wash the filter cake with ethanol 30mL×2; dissolve the filter cake in a mixed solution of 1000mL water and methanol (7:1), stir to dissolve; add seed crystals, control the temperature at 10°C, and stand for crystallization for 3h , filtered; the filtrate was washed with 30 mL of ethanol × 2, and dried in vacuum at 35° C. for 30 min to obtain 15.02 g of cephradine compound in 1 / 5 water.

[0039] The X-ray powder diffraction pattern has characteristic diffraction peaks at diffraction angles 2θ of 7.26°, 10.99°, 14.55°, 16.27°, 17.82°, 19.36°, 20.20°, 22.05°, and 22.92°. The rel...

Embodiment 3

[0042] Embodiment 3: the preparation of 1 / 2 water cephradine compound

[0043] Dissolve 10.5 g of crude cephradine in 100.5 g of water, control the temperature in a water bath at 40 ° C, add 0.5 g of activated carbon, stir and adsorb for 30 min, and filter; adjust the pH value of the filtrate to 6.2 with sulfuric acid; slowly add the dissolution agent trichloride to the above solution Methane, filter, wash the filter cake with ethanol 30mL×2; dissolve the filter cake in a mixed solution of 700mL water and methanol (6:1), stir and dissolve; add seed crystals, control the temperature at 10°C, and stand for crystallization for 3h , filtered; the filtrate was washed with 30 mL of ethanol × 2, and dried in vacuum at 30° C. for 35 min to obtain 10.01 g of cephradine compound in 1 / 5 water.

[0044] The X-ray powder diffraction pattern has characteristic diffraction peaks at diffraction angles 2θ of 7.23°, 10.97°, 14.54°, 16.26°, 17.82°, 19.36°, 20.20°, 22.03°, and 22.92°. The relativ...

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Abstract

The invention discloses a cefradine compound containing half water and a preparation method thereof. Each mole of cefradine comprises a half mole of water. The cefradine compound has characteristic peaks at the positions with the X-ray diffraction spectrum diffraction angle 2 theta of 7.25+ / -0.2 degrees, 10.98+ / -0.2 degrees, 14.53+ / -0.2 degrees, 16.28+ / -0.2 degrees, 17.80+ / -0.2 degrees, 19.38+ / -0.2 degrees, 20.21+ / -0.2 degrees, 22.06+ / -0.2 degrees and 22.90+ / -0.2 degrees. A crude cefradine product is dissolved in water and adsorbed by activated carbon, and a dissolving and precipitation agentis added for crystallization to obtain a cefradine crystal; the crystal is dissolved in a mixed solution of water and methanol, seed crystals are added, and crystallization is performed to obtain thecefradine compound containing half water. The operation is simple, reactants are easy to obtain, the reaction conditions are mild, and the yield is high. The cefradine compound containing half water has great particle size distribution, high fluidity, low impurity content, high stability and a wider application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering pharmaceutical crystallization, and relates to a 1 / 2 water cephradine compound and a preparation method thereof. Background technique [0002] Cefradine (Cefradine) belongs to the first generation cephalosporins, the chemical name is (6R,7R)-7-[(R)-2-amino-2-(l,4-cyclohexadien-1-yl)acetamido ]-3-methyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid. The structural formula is as follows: [0003] [0004] Cefradine is a semi-synthetic cephalosporin antibiotic successfully researched by Bristol-Myers Squibb in 1972, and entered the pharmaceutical market in the 1970s. Cefradine has good curative effect and high safety in clinical treatment of respiratory tract infection, urinary tract infection, skin and soft tissue infection, gastrointestinal infection, bone and joint infection, sepsis, endocarditis, etc., and is widely used in clinical practice . [0005] At present...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/22A61K31/545A61P31/00
Inventor 郝志艳
Owner 陕西顿斯制药有限公司
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