Method for extracting mycophenolic acid

A technology of mycophenolic acid and sulfide, applied in the field of medicinal chemistry, can solve problems such as difficult to remove color, achieve the effects of improving quality, reducing harm and environmental pollution, and improving yield

Active Publication Date: 2014-02-12
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The above method of extracting and refining mycophenolic acid can easily obtain purple mycophenolic acid during use, and once mycophenolic acid is colored, it is difficult to remove the color

Method used

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  • Method for extracting mycophenolic acid
  • Method for extracting mycophenolic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Under stirring, add 3.12g (0.01mol / L) of sodium sulfide to 4L of mycophenolic acid fermentation broth (unit: 4563.2ug / ml), adjust the pH to 9.0 with 3N sodium hydroxide, filter, discard the filter residue, and add 800ml of butyl acetate, adjusted to pH 4.5 with 3N hydrochloric acid, and extracted; the water phase was extracted with 300ml of butyl acetate for the second time, the organic phase was combined, concentrated, set to 200ml, left standing, cooled to 7°C for crystallization, and kept warm After 4 hours, the crystals were separated to obtain the crude product. The crude product was dissolved in 150ml of ethanol, decolorized by adding 1.0g of activated carbon, heated to filter, fixed to 150ml, cooled to 3°C for recrystallization, kept for 4 hours, separated and crystallized, and dried in vacuum to obtain 13.83g of white mycophenolic acid product. The HPLC purity is 99.67%, the calculated content is 99.02%, and the calculated yield is 75.03%.

Embodiment 2

[0068] Under stirring, add 1.56g (0.005mol / L) of sodium sulfide to 4L of mycophenolic acid fermentation broth (unit: 4623.7ug / ml), adjust the pH to 9.0 with 3N sodium hydroxide, filter, discard the filter residue, and add 800ml of butyl acetate, adjusted to pH 4.5 with 3N hydrochloric acid, and extracted; the water phase was extracted with 300ml of butyl acetate for the second time, the organic phase was combined, concentrated, set to 200ml, left standing, cooled to 7°C for crystallization, and kept warm After 4 hours, the crystals were separated to obtain the crude product. The crude product was dissolved in 150ml of ethanol, decolorized by adding 1.0g of activated carbon, heated to filter, set the volume to 150ml, cooled to 3°C for recrystallization, kept for 4 hours, separated and crystallized, and dried in vacuum to obtain 13.96g of white mycophenolic acid product. The HPLC purity was 99.56%, the calculated content was 99.13%, and the calculated yield was 74.82%.

Embodiment 3

[0070] Under stirring, add 15.6g (0.05mol / L) of sodium sulfide to 4L of mycophenolic acid fermentation broth (unit: 4587.9ug / ml), adjust the pH to 9.0 with 3N sodium hydroxide, filter, discard the filter residue, and add acetic acid to the filtrate 800ml of butyl ester was adjusted to pH 4.5 with 3N hydrochloric acid for extraction; the water phase was extracted for the second time with 300ml of butyl acetate, the organic phase was combined, concentrated, and the volume was adjusted to 200ml, left to stand, cooled to 7°C for crystallization, and kept warm After 4 hours, the crystals were separated to obtain the crude product. The crude product was dissolved in 150ml of ethanol, decolorized by adding 1.0g of activated carbon, heated to filter, set the volume to 150ml, cooled to 3°C for recrystallization, kept for 4 hours, separated and crystallized, and dried in vacuum to obtain 13.78g of white mycophenolic acid product. The HPLC purity is 99.54%, the calculated content is 99.0...

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Abstract

The invention relates to a method for extracting mycophenolic acid. The method comprises the step of extracting mycophenolic acid from a mycophenolic acid fermentation broth, wherein sulfide is used for inhibiting oxidation and / or complexing of the mycophenolic acid. By the method provided by the invention, the quality and condition of the mycophenolic acid product can be improved.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for extracting mycophenolic acid. Background technique [0002] Mycophenolic acid (also known as mycophenolic acid, English name: mycophenolic acid), its chemical name is E-4-methyl-6-(1,3-dihydro-7-methyl-4-hydroxy-6- Methoxy-3-oxo-5-isobenzofuryl)-4-hexenoic acid, the molecular formula is C 17 h 20 o 6 , the molecular weight is 320.34, the CAS number is 24280-93-1, and its structural formula is: [0003] [0004] Mycophenolic acid is white or off-white crystalline powder, soluble in methanol and ethanol, slightly soluble in ether and chloroform, hardly soluble in benzene and toluene, almost insoluble in cold water. [0005] Mycophenolic acid was discovered and isolated in Penicillium metabolites in 1893, and its derivatives, sodium mycophenolate mofetil and mycophenolate mofetil, have antitumor properties. [0006] As the main immunosuppressant, m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88
CPCC07D307/88
Inventor 彭平郭萍王先文张洪兰
Owner NEW FOUNDER HLDG DEV LLC
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