1/4 water cefoxitin sodium compound

A technology of cefoxitin sodium and its compound, which is applied in the field of 1/4 water cefoxitin sodium compound and its preparation, and can solve the problems of backward preparation method, instability between batches, poor stability, etc.

Inactive Publication Date: 2018-12-28
梁怡
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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 cefoxitin sodium 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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  • 1/4 water cefoxitin sodium compound
  • 1/4 water cefoxitin sodium compound
  • 1/4 water cefoxitin sodium compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: Preparation of 1 / 4 cefoxitin sodium compound

[0033] making process:

[0034] (1) Dissolve 25.71g of cefoxitin acid in 50mL of water, stir to dissolve, control the temperature at 0-5°C, add 4.0mL of triethylamine dropwise, stir well; add 0.21g of activated carbon for decolorization, filter, and wash with a small amount of water Filter cake; dropwise add a solution of 15.21 g of sodium isooctanoate and 45 mL of ethanol to the filtrate, after the addition is completed, stir, slowly add 25 mL of acetone, and an off-white solid precipitates; filter, and dry under vacuum at 40°C to obtain 26.36 g of crude cefoxitin sodium ;

[0035] (2) Dissolve 26.36 g of the crude product of cefoxitin sodium in 50 mL of water, slowly add 25 mL of acetone to it, control the temperature at 0 to 3° C., and let stand for crystallization for 1.5 h; filter, and wash the filtrate with 40 mL of acetone × 2, After vacuum drying at ℃ for 55 min, 25.79 g of 1 / 4 cefoxitin sodium compo...

Embodiment 2

[0040] Embodiment 2: Preparation of 1 / 4 cefoxitin sodium compound

[0041] making process:

[0042] (1) Dissolve 25.69g of cefoxitin acid in 50mL of water, stir to dissolve, control the temperature at -5~0°C, add 4.0mL of triethylamine dropwise to it, and stir well; add 0.24g of activated carbon for decolorization, filter, and use a small amount of Wash the filter cake with water; add dropwise a solution of 5.54 g of sodium hydroxide and 17 mL of ethanol to the filtrate, after adding, stir, slowly add 25 mL of acetone, and a off-white solid precipitates; filter, and dry in vacuo at 35°C to obtain crude cefoxitin sodium 26.53 g;

[0043] (2) Dissolve 26.53g of crude cefoxitin sodium in 50mL of water, slowly add 25mL of acetone to it, control the temperature at 5-8°C, let stand for crystallization for 2h; Vacuum dried for 55 minutes to obtain 25.68 g of 1 / 4 cefoxitin sodium compound.

[0044] The powder X-ray diffraction pattern has characteristic diffraction peaks at the dif...

Embodiment 3

[0048] Embodiment 3: Preparation of 1 / 4 cefoxitin sodium compound

[0049] making process:

[0050] (1) Dissolve 25.65g of cefoxitin acid in 50mL of water, stir to dissolve, control the temperature at 5-8°C, add 4.0mL of triethylamine dropwise, and stir well; add 0.18g of activated carbon for decolorization, filter, and wash with a small amount of water Filter cake; dropwise add the solution formed by 15.24 g of sodium isooctanoate and 45 mL of ethanol to the filtrate, after the addition is completed, stir, slowly add 25 mL of acetone, and an off-white solid precipitates; filter, and dry in vacuo at 45°C to obtain 26.57 g of crude product of cefoxitin sodium ;

[0051] (2) Dissolve 26.57 g of the crude product of cefoxitin sodium in 50 mL of water, slowly add 25 mL of acetone to it, control the temperature at -3 to 0° C., let stand for crystallization for 2 h; filter, wash the filtrate with 40 mL of acetone × 2, and ℃ vacuum drying for 55min to obtain 1 / 4 cefoxitin sodium co...

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Abstract

The invention discloses a 1 / 4 water cefoxitin sodium compound and a preparation method thereof. Each mole of the cefoxitin sodium contains 1 / 4 mole of water. The preparation method is simple, reactants are easy to obtain, reaction conditions are mild, and the yield is high. The 1 / 4 water cefoxitin sodium compound has good particle size distribution, good fluidity, low impurity content, thermodynamic stability and wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering medicine crystallization, and relates to a 1 / 4 hydrocefoxitin sodium compound and a preparation method thereof. Background technique [0002] Cefoxitin Sodium (Cefoxitin Sodium) is developed by American Merck Company, CAS No. 33564-30-6, molecular formula C 16 h 16 N 3 NaO 7 S 2 , the molecular weight is 449.43, and the chemical name is (6R,7S)-3-(carbamoyloxymethyl)-7-methoxy-8-oxo-7-[2-(2-thienyl)acetamido] -5-Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt, its structural formula is as follows: [0003] [0004] Cefoxitin sodium is a new type of antibiotic produced by semi-synthesis of methoxycephalosporin C produced by Streptomyces. It kills bacteria by inhibiting the synthesis of bacterial cell walls. Cefoxitin sodium, as a second-generation cephalosporin antibiotic, has a broader antibacterial spectrum than the first-generation cephalosporins. The drug ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/57C07D501/04A61K31/546A61P31/04
CPCC07B2200/13C07D501/04C07D501/57
Inventor 梁怡
Owner 梁怡
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