Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of propofol tenofovir lactose impurity

A technology of tenofovir and propofol, applied in the field of pharmaceutical impurity preparation, can solve the problems of no literature report TAF lactose-binding impurity preparation method and the like, and achieve the effects of simple synthesis method, improved quality and easy operation

Pending Publication Date: 2022-03-18
LONZEAL PHARMA
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] It is known that primary and secondary amines react with lactose to form lactose-bound impurities (Maillard L.R., Comptes Rendus, 1912; 154(2):66; Colaco C., Collett M., Roser B., Chem Oggi, 1996; 14 : 32), but there is no bibliographical report TAF lactose binding impurity preparation method

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
  • Preparation method of propofol tenofovir lactose impurity
  • Preparation method of propofol tenofovir lactose impurity
  • Preparation method of propofol tenofovir lactose impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Tenofovir alafenamide (30g) and dimethyl sulfoxide (315mL, moisture content: 0.05%) were added to a 500mL reaction flask, stirred into lactose (86g), and reacted at a temperature of 90-95°C for 35 hours. The reaction liquid was distilled off under reduced pressure to remove dimethyl sulfoxide to obtain a crude product, which was purified with a preparative column, and the preparation conditions were as follows:

[0031] Octadecyl bonded silica gel was used as the stationary phase, mobile phase A: ammonium bicarbonate solution, and mobile phase B: acetonitrile. The gradient elution conditions are as follows:

[0032] Time(min) mobile phase A mobile phase B 0 70％ 30％ 21 50％ 50％ 21.5 5％ 95％ 26 5％ 95％ 26.5 90％ 10％ 30.5 90％ 10％

[0033] The obtained preparation solution was freeze-dried to obtain TAF lactose-binding impurities with an HPLC purity of 97.2%.

[0034] Data Analysis of TAF Lactose Binding Impurity Structure...

Embodiment 2

[0039] Add tenofovir alafenamide (20g) and N,N-dimethylformamide (200mL, water content: 0.02%) into the reaction flask, stir and add lactose (57g), and react at a temperature of 90-95°C for 40 hours , the reaction solution was distilled off under reduced pressure to remove N,N-dimethylformamide to obtain a crude product.

[0040] The crude product was purified by a preparative column, the preparation conditions were the same as in Example 1, and the obtained preparation solution was freeze-dried to obtain TAF lactose-bound impurities with an HPLC purity of 95.6%.

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 relates to the technical field of preparation of medicine impurities, and provides a preparation method of a propofol tenofovir lactose impurity, and the propofol tenofovir lactose impurity is N6-[2, 3-dihydroxy-5-hydroxymethyl-4-(3, 4, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5- The invention relates to a preparation method of tenofovir disoproxil, which is characterized in that the tenofovir disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil disoproxil S2, heating, carrying out condensation reaction with lactose, and distilling to remove the organic solvent, so as to obtain a crude product; and S3, purifying the crude product to obtain the propofol tenofovir lactose impurity. According to the technical scheme, the quality of the propofol fumarate tenofovir standard product is improved.

Description

technical field [0001] The invention relates to the field of preparation of pharmaceutical impurities, in particular to a method for preparing tenofovir alafenamide lactose impurities. Background technique [0002] Tenofovir alafenamide fumarate, English name Tenofovir Alafenamide Fumarate (TAF), is a nucleic acid reverse transcriptase inhibitor developed by Gilead Sciences of the United States. Approved for marketing, it is clinically used for the treatment of chronic hepatitis B; the compound variety Bitovil, approved by NMPA in 2019, is clinically used for the treatment of HIV (HIV) infection. It has been less than two years since it was launched on the market, and its sales in 2020 reached 7.259 billion US dollars, setting a single-drug sales record for AIDS drugs. [0003] TAF and tenofovir disoproxil fumarate (TDF), the most commonly used hepatitis B drug, are both prodrugs of tenofovir (TFV). The antiviral effect, thus greatly reducing the risk of nephrotoxicity and...

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 Applications(China)
IPC IPC(8): C07H1/00C07H1/06C07H19/16G01N33/15
CPCC07H1/00C07H1/06C07H19/16G01N33/15
Inventor 杨志龙王少宾翟家豪巩洪举冯雅慧周玉谷杰
Owner LONZEAL PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com