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Method for preparing cucurbitacine D by hydrolyzing cucurbitacine B

A technology for cucurbitacin and hydrolyzate, applied in the field of medicine, can solve the problems of single source of cucurbitacin D and low purity, and achieve the effects of easy control of reaction, simple and easy method, and high yield

Inactive Publication Date: 2014-05-21
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the single source and low purity of cucurbitacin D, the purpose of the present invention is to provide a method for preparing cucurbitacin D by hydrolysis of cucurbitacin B

Method used

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  • Method for preparing cucurbitacine D by hydrolyzing cucurbitacine B
  • Method for preparing cucurbitacine D by hydrolyzing cucurbitacine B

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Preparation of Cucurbitacin D by Hydrolysis of Cucurbitacin B

[0028] Reaction conditions:

[0029] Cucurbitacin B The organic phase water box pH of aqueous phase organic phase water phase volume ratio temperature reflex Reaction time 100mg 95% ethanol NaOH solution 12 50:50 60℃ 120 minutes

[0030] Weigh 200 mg of cucurbitacin B, dissolve it completely with 20 ml of 95% ethanol, add 20 ml of NaOH solution with a pH value of 12, react at 60°C for 120 min, then stop the reaction in an ice bath, and add 40 ml of The hydrolyzate was extracted with ethyl acetate, and the ethyl acetate was removed by rotary evaporation at 40°C to obtain the desired hydrolyzate.

Embodiment 2

[0031] Example 2: Preparation of Cucurbitacin D by Hydrolysis of Cucurbitacin B

[0032] Reaction conditions:

[0033] Cucurbitacin B The organic phase water box pH of aqueous phase organic phase water phase volume ratio temperature reflex Reaction time 100mg 95% ethanol NaOH solution 10 50:50 60℃ 120 minutes

[0034] Weigh 200 mg of cucurbitacin B, dissolve it completely with 20 ml of 95% ethanol, add 20 ml of NaOH solution with a pH value of 10, react at 60°C for 120 min, then stop the reaction in an ice bath, and add 40 ml of The hydrolyzate was extracted with ethyl acetate, and the ethyl acetate was removed by rotary evaporation at 40°C to obtain the desired hydrolyzate.

Embodiment 3

[0035] Example 3: Preparation of Cucurbitacin D by Hydrolysis of Cucurbitacin B

[0036] Reaction conditions:

[0037] Cucurbitacin B The organic phase water box pH of aqueous phase organic phase water phase volume ratio temperature reflex Reaction time 100mg 95% ethanol NaOH solution 14 50:50 60℃ 120 minutes

[0038] Weigh 200 mg of cucurbitacin B, dissolve it completely with 20 ml of 95% ethanol, add 20 ml of NaOH solution with a pH value of 14, react at 60°C for 120 min, then stop the reaction in ice bath, add 40 ml of The hydrolyzate was extracted with ethyl acetate, and the ethyl acetate was removed by rotary evaporation at 40°C to obtain the desired hydrolyzate.

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Abstract

The invention discloses a method for preparing cucurbitacine D by hydrolyzing cucurbitacine B. The method is simple and easy to implement, and only comprises the steps of (1) dissolving the cucurbitacine B in a good solvent to obtain an organic phase, (2) preparing an alkali liquor having a pH value greater than 9 and / or a buffer solution to obtain a water phase, (3) adding the water phase to the organic phase, and stirring evenly to obtain a reaction solution proportioned in the organic phase and the water phase, (4) reacting the reaction solution at a temperature above 20 DEG C, and then stopping reacting in an ice bath, and (5) adding an isometric ethyl acetate extraction hydrolysis product to the reaction solution in which the reaction is stopped, and carrying out rotary evaporation at 40 DEG C so that the ethyl acetate volatilizes, thus obtaining the desired hydrolysis product. The method solves the problem of single source of the cucurbitacine D.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular to a method for preparing cucurbitacin D by hydrolyzing cucurbitacin B. Background technique [0002] Cucurbitacins are a class of highly oxidized tetracyclic triterpenoids extracted from plants, and more than 40 kinds have been discovered so far. In ancient my country, the traditional Chinese medicine melon stalk was used to treat jaundice, and it can induce vomiting and eliminate phlegm. It can be used to treat severe water evil, edema of limbs, cough and asthma, and those who accidentally ingest poisons that have not yet been absorbed in the gastric cavity. This shows that cucurbitacins have a long history of curing diseases and saving lives in our country. Most of these components exist in Cucurbitaceae plants, and some of them exist in other plants. At present, the cucurbitacin approved for production in my country is also called cucurbitacin BE, which is the extract of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 邓意辉程晓波王春玲佘振南
Owner SHENYANG PHARMA UNIVERSITY
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