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
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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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