Purification process of L-alpha-glycerophosphoryl choline
What is AI technical title?
AI technical title is built by PatSnap AI team. It summarizes the technical point description of the patent document.
A technology of glycerol phosphorylcholine and process, which is applied in the new process field of purification of L-α-glycerophosphorylcholine crude product, can solve the problems of environmental pollution, large consumption of silica gel, increased cost, etc., and achieve process improvement and small consumption , easy recycling effect
Inactive Publication Date: 2015-02-18
合肥创新医药技术有限公司
View PDF7 Cites 11 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Simultaneously because adopted the mixed solvent of four kinds of solvents of acetone, methanol, water, glacial acetic acid as eluent, also not easy to realize recycling
The use of a large amount of solvent and silica gel not only greatly increases the cost, but also causes environmental pollution. Therefore, this process will not be able to realize industrial production in the end.
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
Click on the blue label to locate the original text in one second.
Reading with bidirectional positioning of images and text.
Smart Image
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0046] 8g of crude L-α-glycerophosphorylcholine was removed by ion exchange resin mixed with strong acid type (001×7) and strong base type (201×7) (mass ratio strong acid type: strong base type=1:2) Salt, eluted with deionized water, dried, added 24mL of absolute ethanol to the dried product, started stirring, heated to reflux and clarified, cooled to 0-5°C, added seed crystals, kept at this temperature for 2 hours for crystallization, A large amount of white solids were precipitated, filtered, and vacuum-dried to obtain 6.5g of white powdery L-α-glycerophosphorylcholine, which was detected by HPLC-ELSD as figure 2 , chemical purity 99.8%, mp: 142~145℃, 【α】 D 20 =-2.8°(C=10,H 2 0, pH=5.8). H NMR spectrum ( 1 H NMR) spectrum as figure 1 , 1 H NMR (400MHz,D 2 O): 3.26(s,9H), 3.91~3.78(m,3H), 3.68~3.52(m,4H), 4.26(s,2H).
Embodiment 2
[0048] 8g of crude L-α-glycerophosphorylcholine was removed by ion exchange resin mixed with strong acid type (001×7) and strong base type (201×7) (mass ratio strong acid type: strong base type=1:2) Salt, elute with deionized water, dry, add 32mL of anhydrous isopropanol to the dried product, start stirring, heat to reflux and clarify, cool down to 0-5°C, add seed crystals, keep warm and crystallize at this temperature After 2 hours, a large amount of white solids precipitated, filtered, and dried in vacuum to obtain 6.8 g of white powder L-α-glycerophosphorylcholine, which was detected by HPLC-ELSD with a chemical purity of 99.7%, mp: 142-145°C, [α] D 20 =-2.8°(C=10,H 2 0, pH=5.8).
Embodiment 3
[0050] 8g of crude L-α-glycerophosphorylcholine was desalinated by ion exchange resin (mass ratio strong acid type: strong base type=1:2) of strong acid type (001×7) and strong base type (201×7) , eluted with deionized water, dried, added 40mL of anhydrous n-butanol to the dried product, started stirring, heated to reflux and clarified, lowered the temperature to 0-5°C, added seed crystals, kept warm and crystallized at this temperature for 2 After hours, a large amount of white solids precipitated, filtered, and dried in vacuum to obtain 7.3g of white powder L-α-glycerophosphorylcholine, which was detected by HPLC-ELSD with a chemical purity of 99.5%, mp: 142-145°C, [α] D 20 =-2.8°(C=10,H 2 0, pH=5.8).
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
Property
Measurement
Unit
purity
aaaaa
aaaaa
Login to View More
Abstract
The invention discloses a new process for crystallizing L-alpha-glycerophosphoryl choline (L-alpha-GPC). The process comprises the following steps: firstly, dissolving the crude product L-alpha-glycerophosphoryl choline in an alcoholsolvent, heating to reflux, cooling to the range of 0-5 DEG C, adding seed crystals and preserving heat for crystallization, thereby obtaining the glycerophosphoryl choline crystallized product; filtering and drying the crystallized product to obtain the white crystalpowder of L-alpha-glycerophosphoryl choline having the purity of more than 99.5%. Compared with the prior art, the new process for crystallizing L-alpha-GPC is greatly improved by adopting the crystallization method instead of the column chromatography in the prior art; the single crystallizationsolvent is low in use amount and easy to recovery; the white crystalpowder of L-alpha-glycerophosphoryl choline having the purity of more than 99.5% can be obtained; the process is capable of better meeting the environmental protection requirements, and finally, industrial production can be realized.
Description
technical field [0001] The invention relates to the field of separation and purification of chiral drug L-alpha-glycerophosphorylcholine, in particular to a new purification process of L-alpha-glycerophosphorylcholine crude product prepared by a chemical total synthesis method. Background technique [0002] L-α-glycerophosphorylcholine (English name L-α-glycerophosphorylcholine, hereinafter referred to as GPC), as a choline precursor, is clinically used in the treatment of cerebrovascular diseases, such as a drug for the treatment of Alzheimer's disease. In foreign countries, GPC has been developed into a health product and sold on the market, mainly used to improve the memory of teenagers. In addition, in addition to the application in the field of medicine and health products, GPC can also be used as a whitening ingredient in the field of cosmetics, and as a food additive in some functional foods. Its structural formula is as follows: [0003] [0004] The research on...
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
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to View More