Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation process of mycophenolate mofetil

A technology of mycophenolate morphinate and mycophenolic acid, which is applied in the field of preparation of mycophenolate morphinate, can solve the problems of long time and high reaction temperature, achieve the effect of low reaction temperature and solve the problem of product color

Active Publication Date: 2010-05-12
LIVZON NEW NORTH RIVER PHARMA
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

European patent EP281713B1 adopts the indirect esterification method, and the product has color problems; the preparation method of US patent No.5247083 has high reaction temperature and long time, and the product color also has problems

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 process of mycophenolate mofetil
  • Preparation process of mycophenolate mofetil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 30ml of tetrahydrofuran and 10g of mycophenolic acid into a reactor with a reflux cooler, heat to about 50°C, stir mechanically until completely dissolved, then add 11.5ml of morpholine ethanol into the reactor, and then put 0.8 g catalyst zinc oxide; heat to 67°C, reflux for 24 hours, filter to remove the catalyst zinc oxide; evaporate the organic solvent to dryness under reduced pressure to obtain the crude product of mycophenolate mofetil, add 250ml ethyl acetate to dissolve the crude product, and then use 250ml The mass percent concentration is 5% K 2 CO 3 The solution was washed once, and then washed once with 250ml of purified water; concentrated at a temperature of 40°C to a mass percent concentration of 30%, cooled to 10°C, crystallized for 15 hours, and crystals were precipitated; filtered, and then washed with 10ml of cold ethyl acetate , vacuum-dried at a temperature of 40° C. to finally obtain 11.5 g of a fine product with a purity of ≥99.7% (HPLC), and...

Embodiment 2

[0024] A preparation method of mycophenolate morphinate, comprising the steps of:

[0025] (1) Dissolve mycophenolic acid in tetrahydrofuran at a ratio of 1g:2ml in a reactor with a reflux cooler, heat to about 50°C, and stir until dissolved;

[0026] (2) add morpholine ethanol in the ratio of 1:3 by the mol ratio of mycophenolic acid and morpholine ethanol, then add magnesium oxide as catalyst, make the addition quality of catalyst be 5% of mycophenolic acid quality;

[0027] (3) be heated up to 67 ℃, reflux 24 hours;

[0028] (4) filter, remove catalyst, evaporate organic solvent under reduced pressure, obtain mycophenolate mofetil crude product.

[0029] Add ethyl acetate to dissolve the crude product according to the mass ratio of mycophenolate morphinate crude product to ethyl acetate as 1: 15; 2 CO 3 Wash the solution once, then wash once with purified water of 1.5 times the volume of the solution; concentrate in vacuum at 45°C to a concentration of 20% by mass, cool ...

Embodiment 3

[0031] A preparation method of mycophenolate morphinate, comprising the steps of:

[0032] (1) Dissolve mycophenolic acid in tetrahydrofuran at a ratio of 1g:8ml in a reactor with a reflux cooler, heat to about 50°C, and stir until dissolved;

[0033] (2) adding morpholine ethanol in a ratio of 1:2 by the mol ratio of mycophenolic acid and morpholine ethanol, then adding zinc oxide as a catalyst, so that the added quality of the catalyst is 8% of the quality of mycophenolic acid;

[0034] (3) be heated up to 70 ℃, reflux 20 hours;

[0035] (4) filter, remove catalyst, evaporate organic solvent under reduced pressure, obtain mycophenolate mofetil crude product.

[0036] The following steps may also be included:

[0037] Add ethyl acetate to dissolve the crude product according to the mass ratio of mycophenolate morphinate crude product and ethyl acetate as 1: 25; 2 CO 3 Wash the dissolving solution once, then wash once with purified water twice the volume of the dissolving ...

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 present invention discloses preparation process of Mycopenolate mofetil. The preparation process includes the following steps: dissolving mycopenolic acid in tetrahydrofuran inside a reactor withreflux cooler through stirring; adding morpholine, alcohol and catalyst magnesia and / or zinc oxide; heating and refluxing; filtering to eliminate catalyst and decompression evaporating to eliminate organic solvent and obtain crude Mycopenolate mofetil product. The preparation process is simple, and has low reaction temperature, less produced impurity, conversion rate as high as 85 % and product purity not lower than 99.7 %, and easy industrial application.

Description

technical field [0001] The invention relates to a preparation method of mycophenolate morphinate. Background technique [0002] Mycophnolate Mofetil [0003] [0004] It is an antibiotic with mainly immunosuppressive effect, which is a 2-ethyl ester derivative of mycophenolic acid (MPA). In 1896, Gosio discovered mycophenolic acid. In 1913, Alsberg and Black purified it. Later, Mitsuzuki proved that mycophenolic acid Acids have potentially immunosuppressive properties. The antibiotics with immunosuppressive effect approved by the U.S. Food and Drug Administration (FDA) in October 1998 are mainly used for the prevention of organ rejection after kidney and heart transplantation, and can be used in combination with cyclosporine to reduce the latter’s Dosage and toxicity, the mode of action is inhibition of nucleic acid synthesis. Mycophenolic acid can effectively inhibit the activity of inosine monophosphate dehydrogenase non-competitively, thereby hindering the de novo s...

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): C07D307/88
Inventor 杨亚勇陈海煌李长洪任全华
Owner LIVZON NEW NORTH RIVER PHARMA
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com