A kind of method for preparing vindesine from periwinkle

A technology of vinca vinca and periwinkle, which is applied in the field of preparing vinca dioxin, which can solve the problems of high synthetic reaction conditions, difficulty in obtaining vinca dioxin, complicated reaction steps, etc., and achieve simple equipment requirements, short reaction time, and simple method Effect

Active Publication Date: 2018-07-06
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The series of synthetic reaction conditions are demanding, the reaction steps are complicated, and there are many side reactions.
Therefore, it is difficult to obtain high-purity vinblastine, and the content of vinblastine in vinblastine is only about 0.0005%. How to separate a large amount of high-purity vinblastine is a difficult point

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of vinca total alkaloids

[0021] Take 100kg of periwinkle stems and leaves, crush them, add 200L of 70% ethanol-water solution, adjust the pH of the extract solution to 3 with sulfuric acid, soak for 24 hours, filter, and re-extract the filter residue according to the above method, combine the extracts, and recover ethanol under reduced pressure Filter and discard the filter residue. Add 50L of water to the filtrate for dilution, adjust the pH to 9 with ammonia water after dilution, and add 50L of chloroform to it. The layers were separated after standing, and the chloroform layer was collected, and the water layer was extracted once again with 50 L of chloroform. The chloroform layers from the two extractions were combined. After recovering chloroform under reduced pressure, 112 g of total alkaloids of vinca were obtained.

[0022] (2) Preparation of Crude Vinblastine Sulfate

[0023] Install a silica gel column (100-200 mesh) according to the samp...

Embodiment 2

[0033] (1) Preparation of vinca total alkaloids

[0034] Stems and leaves of periwinkle 100kg, crushed and added to 200L of 70% ethanol-water solution, adjusted to pH=3 of the extract with sulfuric acid, soaked for 24 hours, filtered, and the filter residue was extracted once again according to the above method, combined with the extract, recovered ethanol under reduced pressure and filtered , and the filter residue was discarded. Add 50L of water to the filtrate for dilution, adjust the pH to 9 with ammonia water after dilution, and add 50L of chloroform to it. The layers were separated after standing, and the chloroform layer was collected, and the water layer was extracted once again with 50 L of chloroform. The chloroform layers from the two extractions were combined. After recovering chloroform under reduced pressure, 116 g of total alkaloids of vinca were obtained.

[0035](2) Preparation of Crude Vinblastine Sulfate

[0036] Install a silica gel column (100-200 mesh...

Embodiment 3

[0046] (1) Preparation of vinca total alkaloids

[0047] 300kg of periwinkle stems and leaves, crushed and added 600L of 70% ethanol-water solution, adjusted the pH of the extract solution to 3 with sulfuric acid, soaked for 24 hours, filtered, and re-extracted the filter residue according to the above method, combined the extracts, recovered ethanol under reduced pressure and filtered , and the filter residue was discarded. Add 150L of water to the filtrate for dilution, adjust the pH to 9 with ammonia water after dilution, and add 150L of chloroform to it. The layers were separated after standing, and the chloroform layer was collected, and the water layer was extracted once again with 150 L of chloroform. The chloroform layers from the two extractions were combined. After recovering chloroform under reduced pressure, 350 g of total alkaloids of vinca were obtained.

[0048] (2) Preparation of Crude Vinblastine Sulfate

[0049] Install 3 silica gel columns (100-200 mesh)...

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Abstract

The invention discloses a method for preparing eldisine from Catharanthus roseus. The method comprises the following steps: (1) preparation of Catharanthus roseus total alkaloid; (2) preparation of vinblastine sulfate crude product; (3) preparation of vinblastine sulfate pure product; (4) preparation of vinblastine hydrazide; and (5) preparation of eldisine. The method is simple to technique and convenient to operate; and the production keypoints are easy to control, so the method is suitable for industrial production. The silica gel has the advantages of low cost and simple equipment requirements. The vinblastine sulfate refinement process after salification is simple and convenient; and the refined vinblastine sulfate has the advantages of high content and high yield. In the eldisine preparation process, the azidation reaction and hydrolysis reaction are carried out in one reactor, so the reaction time is short, and the amount of reaction byproducts is smaller. After the reaction, the eldisine has the advantages of higher content and high yield.

Description

technical field [0001] The invention relates to the fields of organic synthesis chemistry and natural medicinal chemistry, in particular to a process for preparing vindesine from periwinkle flowers. Background technique [0002] Two of the four nitrogen atoms of vindesine are alkaline and can form salts with appropriate acids. Vindesine Sulfate is easily soluble in water and alcohol, but insoluble in n-hexane. It is a white or nearly white powder, which needs to be sealed, protected from light, and stored in a freezer. Vindesine is a cycle-specific drug that mainly acts on cells in metaphase (M phase) of mitosis. Mainly by inhibiting the polymerization of tubulin, it hinders the formation of the spindle, so that the cells stop and mitotic metaphase. Clinically, vindesine is widely used in the blood system such as acute lymphoblastic leukemia, lymphoma, multiple myeloma, and chronic myeloid blast. [0003] Vindesine (Videsine) is generally synthesized by a series of chemic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D519/04
CPCC07D519/04
Inventor 陈洪亮袁诚黄建军陈卫林许文东李金华
Owner GUANGZHOU HANFANG PHARMA
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