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

Process for large-scale preparation of pravastatin sodium D-type crystal

A technology of pravastatin sodium and a process is applied in the field of large-scale preparation of pravastatin sodium D-type crystals, and can solve the problems of yellowish color of pravastatin sodium D-type crystals, low crystal transformation efficiency, and unsuitability for industrial scale-up. , to achieve the effect of simple and easy process, high crystal form conversion rate and simple preparation method

Active Publication Date: 2016-09-21
GUANGDONG BLUE TREASURE PHARMA
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above two methods are all to convert the pravastatin sodium in a certain crystal form into D-type pravastatin sodium crystals under atmospheric pressure, which is not suitable for industrial amplification; meanwhile, the pravastatin sodium D prepared by the above method is The color of the crystal is yellow or gray, the appearance of the product is not good, and the effective rate of crystal transformation is low, and the impurity content is high

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
  • Process for large-scale preparation of pravastatin sodium D-type crystal
  • Process for large-scale preparation of pravastatin sodium D-type crystal
  • Process for large-scale preparation of pravastatin sodium D-type crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation of embodiment 1 pravastatin sodium type D crystal

[0031] S1: Take pravastatin sodium crystals, add butanol with a water content of 5% at a liquid-solid ratio of 0.1mL / g at a temperature of 12°C, and ultrasonically mix for 8 minutes at an ultrasonic power of 750W to prepare into a mixed slurry;

[0032] S2: Put the mixed slurry described in S1 in a vacuum drying oven, raise the temperature to 65°C, and pass high-purity nitrogen gas for 12 hours while vacuuming, and keep the vacuum value at -0.40MPa;

[0033] S3: Stop feeding high-purity nitrogen, keep the temperature at 60°C, adjust the vacuum value to -1.0MPa, and dry for 12 hours to obtain the product.

[0034] The prepared product is a white crystal, and its PXRD spectrum is as follows: figure 1 As shown, there are obvious characteristic peaks at diffraction angles 2θ°=3.8, 6.5, 9.8 and 17.0°, which are pravastatin sodium type D crystals, and it can be clearly seen from the PXRD pattern that except...

Embodiment 2

[0035] The preparation of embodiment 2 pravastatin sodium type D crystals

[0036] S1: Take pravastatin sodium crystals, and add an equal volume of acetone and propanol mixed organic solvent with a water content of 3% at a liquid-solid ratio of 0.12mL / g at a temperature of 10°C. Under the condition of 500W, ultrasonically mix for 10min to make a mixed slurry;

[0037]S2: Put the mixed slurry described in S1 in a vacuum drying oven, raise the temperature to 70°C, and pass high-purity nitrogen gas for 10 hours while vacuuming, and keep the vacuum value at -0.90MPa;

[0038] S3: Stop feeding high-purity nitrogen, keep the temperature at 50°C, adjust the vacuum value to -0.95MPa, and dry for 12h to obtain the product.

[0039] The prepared product is a white crystal, and its PXRD spectrum is as follows: figure 2 As shown, there are obvious characteristic peaks at diffraction angles 2θ°=3.7, 6.4, 9.8 and 16.9°, which is a D-type crystal of pravastatin sodium, and it can be clear...

Embodiment 3

[0040] Embodiment 3 Preparation of pravastatin sodium D-type crystal

[0041] S1: Take pravastatin sodium crystals, add propanol with a water content of 10% at a liquid-solid ratio of 0.08mL / g at a temperature of 10°C, and ultrasonically mix for 6 minutes at an ultrasonic power of 600W to prepare into a mixed slurry;

[0042] S2: Put the mixed slurry described in S1 in a vacuum drying oven, raise the temperature to 50°C, and pass high-purity nitrogen gas for 15 hours while vacuuming, and keep the vacuum value at -0.60MPa;

[0043] S3: Stop feeding high-purity nitrogen, keep the temperature at 70°C, adjust the vacuum value to -1.0MPa, and dry for 15 hours to obtain the product.

[0044] The prepared product is a white crystal, and its PXRD spectrum is as follows: image 3 As shown, there are obvious characteristic peaks at diffraction angles 2θ°=3.8, 6.4, 9.8 and 16.9°, which are pravastatin sodium type D crystals, and it can be clearly seen from the PXRD pattern that in addi...

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 a process for large-scale preparation of a pravastatin sodium D-type crystal. The process comprises the following steps: 1) taking a pravastatin sodium crystal, adding an organic solvent according to the liquid-solid ratio of 0.08-0.15 mL / g at a temperature of 10-20 DEG C, and performing ultrasonic uniform mixing for 5-10 minutes to prepare mixed slurry; 2) putting the mixed slurry into a vacuum drying oven, raising the temperature to 50-70 DEG C, introducing high-purity nitrogen for 10-15 hours while performing vacuum pumping treatment, and keeping a vacuum value to be minus 0.90 - minus 0.40 MPa; 3) stopping introduction of the high-purity nitrogen, keeping the temperature at 50-70 DEG C, regulating the vacuum value to minus 0.95 - minus 1.0 MPa, drying for 10-15 hours, and obtaining the pravastatin sodium D-type crystal. The invention provides the process for the large-scale preparation of the pravastatin sodium D-type crystal, a large amount of organic solvents is not required to be used in the preparation process, and a product prepared is the white pravastatin sodium D type crystal and is high in purity.

Description

technical field [0001] The invention relates to a process for large-scale preparation of D-type crystals of pravastatin sodium. Background technique [0002] Solid matter can be divided into crystalline and amorphous according to whether the arrangement of its particles in the structure is periodic. When the substance is crystallized, due to the influence of various factors, the bonding mode in the molecule or between the molecules changes, resulting in a different arrangement of the molecules or atoms of the crystal in the lattice space, forming different crystal structures, that is, different crystal structures. This phenomenon is called polymorphism. Due to the different crystal structures, the interaction forces and binding energies between particles of different crystal forms are also different, and their physical and chemical properties and optical properties are also different, resulting in different stability of different crystal forms. Most drugs have polymorphism...

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): C07C69/33C07C67/52
CPCC07B2200/13C07C67/52C07C69/33
Inventor 陈继敏徐会根黄智勇罗定军李耀荣熊志叶家雄
Owner GUANGDONG BLUE TREASURE 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