Preparation process for homoharringtonine

A technology of homoharringtonine and harringtonine, which is applied in the direction of organic chemistry, can solve the problems of unfavorable industrial production, less seed production, and less storage quantity, so as to improve the actual utilization rate, reduce environmental pollution, and increase yield and the effect of purity

Pending Publication Date: 2021-10-29
泰华天然生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the above method is that it is necessary to use the rhizomes and trunks of the cloverwood as raw materials to prepare homoharringtonine, and the cloverleaf plants are relict species of the Tertiary period, with scattered distribution and small number of preservation, and their population composition Incomplete, less fruiting, low germination rate, very difficult to regenerate, coupled with over-harvesting, many species are endangered or even extinct. The content of the homoharringtonine prepared by the above method is also low, which is unfavorable for industrialized production

Method used

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  • Preparation process for homoharringtonine
  • Preparation process for homoharringtonine
  • Preparation process for homoharringtonine

Examples

Experimental program
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Effect test

Embodiment 1

[0057] A process preparation method of homoharringtonine, the preparation method steps are as follows:

[0058] S1. Select raw materials of Chinese fir twigs and remove impurities;

[0059] S2, pulverizing the treated net material into a 10-20 mesh coarse powder to obtain a three-point fir coarse powder;

[0060] S3. Add 4 times more than 95% methanol to the coarse powder of Chinese fir, extract 3 times, each time for 2 hours, and the temperature is 65°C;

[0061] S4. Combine the three extracts, concentrate under reduced pressure until the relative density of the extract is 1.1 to obtain the extract 1, and the environment for measuring the relative density of the extract is: temperature: 60°C, vacuum degree: 0.03MPa, temperature 55-60°C;

[0062] S5. Add an equivalent amount of 1% HCl aqueous solution to the obtained extract 1, stir and dissolve it for 2 hours, and then adjust the pH to PH=2 with water;

[0063] S6. Leave the acid aqueous solution with PH=2 for 24 hours, cen...

Embodiment 2

[0079] Based on embodiment 1, a kind of process preparation method of homoharringtonine also includes the following steps:

[0080] S10-1. Adjust the pH of the acidic water solution 3 obtained in step S8 in Example 1 to PH=9 with 10% ammonia water, then add an equal amount of chloroform to stir and extract for 5 min, let it stand for 0.5 h, and release the lower chloroform layer after separation , repeat the extraction in this way until no alkaloid is detected in the chloroform, and obtain the chloroform liquid 2 and the acid water liquid 4, and directly discard the acid water liquid 4;

[0081] S10-2, the chloroform solution 2 obtained in step S10-1 was dried with anhydrous sodium sulfate, concentrated under reduced pressure to a relative density of 1.2 (measured at 60°C), the temperature was 55-60°C, and the vacuum degree was 0.03MPa, and the reagent was recovered to obtain the leached Cream 3 (crude torreya).

Embodiment 3

[0083] A process preparation method of homoharringtonine, the preparation method steps are as follows:

[0084] S1. Select raw materials of Chinese fir twigs and remove impurities;

[0085] S2, pulverizing the treated net material into a 10-20 mesh coarse powder to obtain a three-point fir coarse powder;

[0086] S3. Add 3 times more than 95% methanol to the coarse powder of Chinese fir, extract twice, each time for 1 hour, at a temperature of 60°C;

[0087] S4. Combine the three extracts, concentrate under reduced pressure until the relative density of the extract is 1.0 to obtain the extract 1, the environment for measuring the relative density of the extract is: temperature: 60°C, vacuum degree: 0.03MPa, temperature 55-60°C;

[0088] S5. Add an equivalent amount of 1% HCl aqueous solution to the obtained extract 1, stir and dissolve it for 2 hours, and then adjust the pH to PH=3 with water;

[0089] S6. Let the acid aqueous solution with pH=3 stand for 23 hours, centrifug...

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Abstract

The invention discloses a preparation process for homoharringtonine. The preparation process comprises the following steps: selecting a raw material, namely branches of cephalotaxus fortunei, thoroughly removing impurities, crushing the branches, performing extracting with methanol, combining liquid extracts, and carrying out concentrating under reduced pressure to obtain an extract 1; and subjecting the extract 1 to stirring and dissolving, adjusting a pH value, carrying out standing and centrifugation, adding petroleum ether, and carrying out extraction on acid precipitation supernatant multiple times. According to the invention, the content of homoharringtonine in a finally obtained sample is larger than 99%, so yield and purity are greatly improved compared with a traditional technology; only branches and leaves of cephalotaxus chinensis are used as raw materials for preparing homoharringtonine in the preparation method, so industrial production can be carried out on the premise that normal growth of tree species is not affected and the environment is not damaged; used reagents, and namely methanol and chloroform can be effectively recovered and repeatedly utilized in the preparation process, so environmental pollution is reduced to the maximum extent while an actual utilization rate is increased.

Description

technical field [0001] The invention relates to the technical field of medicine preparation, in particular to a preparation method of homoharringtonine. Background technique [0002] Homoharringtonine is an alkaloid isolated from the total alkaloids of Torreya genus. It is a highly effective antineoplastic drug successfully developed in my country. It has been clinically proven to be effective against acute myeloid leukemia Chemicalbook, acute monocytic leukemia, All kinds of acute non-lymphocytic leukemia and chronic myelogenous leukemia, such as leukemia, have good curative effect. It has strong cytotoxicity, and can also cause cardiotoxicity and bone marrow suppression, which limits the increase of chemotherapy dose. [0003] The existing common preparation process of homoharringtonine is to make the rhizome, trunk and bark of the harringtonine into coarse powder, add alcohol to extract, and the obtained solution is separated by column layer with aluminum hydroxide, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/20
CPCC07D491/20
Inventor 柳超
Owner 泰华天然生物制药有限公司
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