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Purification method and preparation method for 4',7-diethyl tectorigenin

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
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

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  • Purification method and preparation method for 4',7-diethyl tectorigenin
  • Purification method and preparation method for 4',7-diethyl tectorigenin
  • Purification method and preparation method for 4',7-diethyl tectorigenin

Examples

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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).

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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

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/40C07D311/36
CPCC07D311/40C07D311/36
Inventor 陈帅袁崇均罗森王笳张磊李利民陈雏吴燕宁楠
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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