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Method for separating out nafcillin acid crystal from nafcillin sodium water solution

A technology of nafcillin sodium and nafcillin acid, which is applied in the direction of organic chemistry, can solve the problems of long drying time at room temperature (24 hours, poor quality of finished products, large environmental pollution, etc., and achieve single extraction agent, short drying time, The effect of less residual solvent

Active Publication Date: 2009-06-17
朗致集团江西医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that it is necessary to add methyl isobutyl ketone first to obtain adhesive precipitation, and then to obtain the finished product through recrystallization. The room temperature drying time is long (about 24 hours), the process is complicated, and the workload is large. About 80% (high performance liquid chromatography analysis), mixed use of various solvents, difficult to recycle, high cost, and large environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add about 1200kg nafcillin sodium aqueous solution and 90kg ethyl acetate into a 2000L reaction tank, start stirring, pass brine into the interlayer to cool down to 0-10°C, add 3% dilute sulfuric acid solution dropwise, acidify to pH=1.5-2.0 ( Acidification time is about 0.5h), precipitate crystals, continue to stir for 1h, filter, wash the crystals with purified water until the pH of the washing solution is 4.0, drain the washed filter cake, smash it into a plate, and put it in a 45-55°C In a vacuum oven, dry to a moisture content of 2.4% to obtain nafcillin acid with a content of 95.25%.

Embodiment 2

[0021] Add about 1200kg nafcillin sodium aqueous solution and 90kg butyl acetate into a 2000L reaction tank, start stirring, pour brine into the interlayer, cool down to 0-10°C, add 5% dilute hydrochloric acid solution dropwise, acidify to pH=1.5~ 2.0, precipitate crystals, continue to stir for 2 hours, filter, wash the crystals with purified water until the pH of the washing solution is 4.0, drain the washed filter cake, grind it into a plate, put it in a vacuum drying oven at 45-55°C, and dry When the water content reaches 2.1%, nafcillin acid is obtained with a content of 96.54%.

Embodiment 3

[0023] Add about 1200kg nafcillin sodium aqueous solution and 100kg n-butanol into a 2000L reaction tank, pass brine into the interlayer, cool down to 0-10°C, start stirring, add 2% phosphoric acid solution dropwise, acidify to pH=1.5-2.0 , to precipitate crystals, continue to stir for 2 hours, filter, wash the crystals with 300L purified water until the pH of the washing solution is 4.0, drain the washed filter cake, crush it and put it on a plate, put it in a vacuum oven at 45-55°C, and dry it When the water content reaches 1.85%, nafcillin acid is obtained with a content of 94.89%.

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PUM

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Abstract

The invention relates to a method for separating out nafcillin acid crystal from a nafcillin sodium aqueous solution, which comprises the following steps: adding one of ethyl acetate, butyl acetate, n-butanol, n-hexane or petroleum ether as an extracting agent into the nafcillin sodium aqueous solution, and dripping an acidifying agent into the solution to make the pH value to be between 1.5 and 2.0 so as to separate out the crystal; and separating out the crystal, washing the crystal by purified water to make the pH value of washing liquor to be 4.0, drying the crystal at a temperature of between 45 and 55 DEG C to ensure that the moisture is below 3 percent to obtain the nafcillin acid crystal. The nafcillin acid crystal separated out by the extracting agent has the advantages of good crystal form, easy filtration, easy drying, less residual solvent in a product, and good quality; and the content of nafcillin acid is more than 93 percent. The crystallization method has the advantages of simple crystallize process, single extracting agent, and easy reclamation.

Description

technical field [0001] The invention relates to a semi-synthetic antibiotic nafcillin sodium, in particular to a method for synthesizing nafcillin acid as an intermediate of nafcillin sodium, in particular to a method for separating nafcillin acid crystals from an aqueous solution of nafcillin sodium. Background technique [0002] Nafcillin sodium is also known as ethoxynaphthylin, new penicillin III, chemical name (2S, 5R)-3,3-dimethyl-6-(2-ethoxy-1-naphthyl)-7-oxidation- 4-Thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid sodium salt monohydrate, molecular formula C 21 h 21 o 5 N 2 SNa·H 2 O, molecular weight 454.49, trade name Unipen, first developed by Wyeth Company of the United States, suitable for penicillin-resistant staphylococcal infections and other penicillin-sensitive bacterial infections, such as: sepsis, endocarditis, empyema, liver abscess, pneumonia, Osteomyelitis etc. [0003] So far, the chemical synthesis method report of relevant nafcillin sodium a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/74
Inventor 陆晨阳刘秀兰李忠华杨秉一李祖文郭剑虹周改平李建侠
Owner 朗致集团江西医药有限公司
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