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Compounding method for chrysoeriol

The technology of a golden eriodroxanthin and a synthetic method is applied in the field of synthesis of golden eriodroxanthin, which can solve the problems of large reaction odor, low cyclization yield, complex post-treatment, etc., and achieves simple steps, simple post-treatment, The effect of easy purification

Inactive Publication Date: 2018-02-13
陕西嘉禾药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses the iodopyridine system, the whole reaction has a big smell, the post-treatment is complicated and the cyclization yield is very low

Method used

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  • Compounding method for chrysoeriol
  • Compounding method for chrysoeriol
  • Compounding method for chrysoeriol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 12g of anhydrous phloroglucinol, 24g of ethyl 3-methoxy-4-hydroxy-benzoylacetate, and 120g of DMSO in a 250ml beaker, heat up and stir in a vacuum for 12 hours, then stop the heating, remove the vacuum and cool to room temperature Then add 200ml of water, stir for 12 hours, and filter to obtain 32g of solid crude eriodine.

[0030] Recrystallize the crude product with 15 times the volume of new ethanol, add 10% of the mass of the crude product to decolorize with activated carbon, remove the activated carbon, concentrate the ethanol to one-fifth of the original volume, place it for crystallization, filter and dry to obtain 98% golden eriodictine 29 grams.

Embodiment 2

[0032] Put 6g of anhydrous phloroglucinol, 12g of 3-methoxy-4-hydroxy-ethyl benzoylacetate, and 60g of DMSO in a 250ml beaker, heat up and stir in a vacuum reaction for 12 hours, then stop heating, remove the vacuum and cool to room temperature Then add 100ml of water, stir for 12 hours, and filter to obtain 15g of solid crude eriodine.

[0033] Recrystallize the crude product with 15 times the volume of new ethanol, add 10% of the mass of the crude product to decolorize with activated carbon, remove the activated carbon, concentrate the ethanol to one-fifth of the original volume, place it for crystallization, filter and dry to obtain 98% golden eriodictine 13 grams.

Embodiment 3

[0035] Put 24g of anhydrous phloroglucinol, 48g of 3-methoxy-4-hydroxy-ethyl benzoylacetate, and 240g of DMSO in a 500ml beaker, heat up and stir in a vacuum for 12 hours, then stop the heating, remove the vacuum and cool to room temperature Then add 400ml of water, stir for 12 hours, and filter to obtain 65g of solid crude eriodine.

[0036] Recrystallize the crude product with 15 times the volume of new ethanol, add 10% of the mass of the crude product to decolorize with activated carbon, remove the activated carbon, concentrate the ethanol to one-fifth of the original volume, place it for crystallization, filter and dry to obtain 98% golden eriodictine 63 grams.

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Abstract

The invention provides a compounding method for chrysoeriol, solving the problems of operation complexity and low yield in the prior art. The compounding method includes mixing anhydrous phloroglucinol with 3-methoxy-4-hydroxy-benzoyl ethyl acetate and dimethyl sulfoxide, heating and stirring the mixture, stopping heating to remove vacuum after complete vacuum reaction, cooling the mixture to roomtemperature, adding water, and performing stirring and filtering to obtain a crude chrysoeriol solid; subjecting the crude chrysoeriol solid to recrystallization by ethyl alcohol, and performing decoloration, concentration, recrystallization, filtration and drying to obtain the refined chrysoeriol. The compounding method has the advantages of simple and convenient procedure, simplicity in post-treatment, high yield of the whole process and applicability to large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for synthesizing golden eriodictine. Background technique [0002] Chrysoriol, chemical name: 3'-methoxy-4',5,7-trihydroxyflavone, molecular formula C 16 h 12 o 6 , the structural formula is: [0003] [0004] Golden erionthizanthin is one of the natural flavonoids, which exists in many plants, such as fresh leaves and roots of Rehmannia glutinosa from Huaiqing, Artemisia baicalensis, Rhizoma chinensis, Honeysuckle, Aurantia chinensis leaves, Sour vine, Physalis Golden Holy Grass Yellow can be isolated from plants such as Asteraceae blue thorns, palm leaves, carrot roots, peony petals, betel nuts, chrysanthemum brain medicinal materials (dry young stems and leaves of chrysanthemum brain), epimedium and winter grass Phytoxanthin, and golden eriodroxanthin is also one of the components that affect the color of peony flowers. [0005] Golden eriodictine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30
CPCC07D311/30
Inventor 郭文华肖金霞赵景辉肖红王晓莹张瑜
Owner 陕西嘉禾药业有限公司
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