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Purification method of loteprednol etabonate

A technique of loteprednol and a purification method, applied in the field of purification of loteprednol, can solve problems such as failure to meet medicinal requirements, difficult removal of impurities and the like

Active Publication Date: 2013-02-06
SHANDONG INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The final product of this process is refined with acetone. Although the purity can reach about 98%, there are still nearly 2% of impurities that are difficult to remove and cannot meet the requirements for medicinal use.

Method used

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  • Purification method of loteprednol etabonate
  • Purification method of loteprednol etabonate
  • Purification method of loteprednol etabonate

Examples

Experimental program
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Effect test

example 1

[0024] Take 50 grams of loteprednol crude product, add it in a 1000 ml four-necked round bottom flask, add 500 ml of absolute ethanol, heat to reflux, the inner temperature is 78.5 ° C, stir and dissolve, cool down slightly, add 25 grams of activated carbon, continue Stir for 10 minutes, heat filter, the filtrate is naturally cooled to room temperature, natural crystallization, after airtight placement for 48 hours, suction filtration, washing with a small amount of ethanol, and vacuum drying at 50°C to obtain 43 grams of loteprednol fine product, the yield is 86%. HPLC detects that the content is 99.6%, and the content of the impurity peaks of related substances is all below 0.1%.

example 2

[0026] Take 50 grams of loteprednol crude product, add it in a 1000 milliliter four-neck round bottom flask, add 600 milliliters of isopropanol, heat to reflux, the inner temperature is 82.5 ℃, after stirring and dissolving, cool down slightly, add 25 grams of activated carbon, continue Stir for 10 minutes, heat filter, the filtrate is naturally cooled to room temperature, natural crystallization, after airtight placement for 48 hours, suction filtration, washing with a small amount of ethanol, and vacuum drying at 50°C to obtain 42 grams of loteprednol fine product, the yield is 84%. HPLC detects that the content is 99.5%, and the content of the impurity peaks of related substances is all below 0.1%.

example 3

[0028] Take 50 grams of loteprednol crude product, add it to a 1000 ml four-necked round-bottomed flask, add 700 ml of anhydrous, heat to reflux, the inner temperature is 64.5°C, stir and dissolve, then cool down slightly, add 30 grams of activated carbon, and continue stirring 10 minutes, hot filtration, filtrate naturally cooled to room temperature, natural crystallization, airtight place after 48 hours, suction filtration, a small amount of ethanol washing, 50 ℃ of vacuum drying, obtain loteprednol fine product 40 grams, yield is 80%, by HPLC Detection, the content is 99.5%, and the content of the impurity peaks of related substances is all below 0.1%.

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Abstract

The invention discloses a purification method of loteprednol etabonate, in particular to a purification method of a steroidal anti-inflammatory drug such as loteprednol etabonate,which is characterized by comprising: alcohol, isopropanol or methanol serves as solvent; a loteprednol etabonate sample is heated and dissolved at the temperature of 50-100 DEG C; active carbon is added into the loteprednol etabonate solution, wherein the ratio of the weight of active carbon to the volume of loteprednol etabonate solution is 1-10%; decolouration is carried out; and cooling and crystallization is carried out to obtain the purpose of purifying the loteprednol etabonate.

Description

technical field [0001] The invention relates to a purification process of steroidal anti-inflammatory drug loteprednol. Background technique [0002] Loteprednol (Loteprednol etabonate) is a new type of corticosteroid anti-inflammatory drug developed by Pharmos Corp., and its chemical name is 17α-[(ethoxyformyl)oxyl]-11β-hydroxyl-3 - Chloromethyl oxoandrost-1,4-diene-17β-carboxylate, the structure is as follows: [0003] [0004] It was first approved by the FDA in 1997 for marketing in the US and in 2000 in the UK. This product is a typical representative of a new type of drug-soft drug, known as a soft drug corticosteroid steroid drug, which has anti-keratitis, various intraocular inflammation and anti-allergic effects, and its systemic toxicity is small. It has been confirmed by pharmacological studies that it has a good development prospect, and the compound preparation with tobramycin has also been listed, and domestic research on this drug has gradually deepened. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J3/00
Inventor 刘宪华张雯任业明孔祥雨赵思太
Owner SHANDONG INST OF PHARMA IND
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