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
View PDF1 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Purification method of loteprednol etabonate
  • Purification method of loteprednol etabonate
  • Purification method of loteprednol etabonate

Examples

Experimental program
Comparison scheme
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%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap