Purification method and preparation method for 4',7-diethyl tectorigenin
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technique for purifying aglycone and its purification method, which is applied in the field of purification of 4′,7-diethylaglycone, which can solve the problems of untrue content, real yield and low purity of the product, and achieve reliable quality Effect
Inactive Publication Date: 2017-05-10
SICHUAN ACAD OF CHINESE MEDICINE SCI
View PDF1 Cites 0 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
However, in its preparation method, the sample does not have the process of dissolving, filtering, and crystallization, but repeatedly elutes with 95% ethanol to remove impurities, and the measurement method is the area normalization method, and its content is not the real content. The real yield and purity are not high, the content determined by HPLC external standard method is 97.23%, and the residue on ignition is 1.2%
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
[0037] Example 1 Preparation of 4′, 7-diethyl shegan aglycon
[0038] Weigh 100g of Shegan aglycon, add 100g of NaOH, 1000mL of 95% ethanol, 200mL of diethyl carbonate, reflux in a water bath for 2 hours, take it out, neutralize with an appropriate amount of 36% hydrochloric acid to pH=1~2, add water, stir and let cool, filter , and dried under reduced pressure at 60°C to obtain a light yellow powder, namely 4',7-diethylsedaglycone, with a yield of 50% and a purity of 60% (HPLC area normalization method).
Embodiment 2
[0039] Example 2 Preparation of 4′, 7-diethyl sheganaglycone
[0040] Weigh 100g of Shegan aglycone, add 100g of NaOH, 1000mL of 95% ethanol, 200mL of ethyl iodide, reflux in a water bath for 30 minutes, take it out, neutralize with an appropriate amount of 36% hydrochloric acid to pH=1~2, add water, stir and let cool, filter, Drying under reduced pressure at 60°C gave a light yellow powder, ie 4',7-diethyl aglycone, with a yield of 75% and a purity of 78% (HPLC area normalization method).
Embodiment 3
[0041] Example 3 Preparation of 4′,7-diethyl shegan aglycon
[0042] Weigh 100g of Shegan aglycone, add 100g of NaOH, 1000mL of 95% ethanol, 200mL of ethyl bromide, reflux in a water bath for 1 hour, take it out, neutralize with an appropriate amount of 36% hydrochloric acid to pH=1~2, add water, stir and let cool, filter, After drying under reduced pressure at 60°C, a light yellow powder was obtained, namely 4',7-diethyl aglycone, with a yield of 70% and a purity of 72% (HPLC area normalization method).
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
Login to view more
Abstract
The invention discloses a method for purifying 4',7-diethyl tectorigenin. The method comprises the following steps: (1) heating and dissolving the 4',7-diethyl tectorigenin in a solvent, performing filtering, and extracting filtrate; (2) adding an anti-solvent anhydrous ethanol into the filtrate; and performing cooling crystallization and filtering; (3) extracting filtered solids, and performing recrystallization by adopting the same solvent in step (1); (4) separating crystals, and performing drying. The invention further provides a method for preparing the 4',7-diethyl tectorigenin. The method comprises the following steps: (A) adding NaOH and an ethylation reagent into a raw material tectorigenin, and performing reaction to obtain a reaction solution; (2) performing acidification to regulate the pH value of the reaction solution to 1 to 2, adding water, and performing filtering and purification to obtain the 4',7-diethyl tectorigenin. According to the purification method and the preparation method, high-purity 4',7-diethyl tectorigenin can be conveniently and effectively prepared by process screening.
Description
technical field [0001] The invention relates to the field of medicines, in particular to a purification method and a preparation method of 4′,7-diethyl schizoglycon. Background technique [0002] Coxsackie virus is an enterovirus, divided into two types, type A and type B. After the virus enters the human body and reproduces in the pharynx and intestinal mucosal cells, it can invade the blood to form viremia, and then spread to other places. Central nervous system, respiratory tract, heart, muscle, skin, etc., can cause aseptic meningitis, rash fever, acute myocarditis and pericarditis, epidemic myalgia, upper flu, herpetic pharyngitis and infant diarrhea Wait. [0003] Currently, there is no clinically effective drug for the treatment of Coxsackievirus. Antiviral drugs such as ribavirin, interferon, nutritional preparations, traditional Chinese medicine Huangqi Shenmai injection and other symptomatic and conservative treatments are commonly used. [0004] Patent CN1017239...
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 
Login to view more