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A kind of vincristine compound impurity and its preparation method and application

A vincristine and compound technology, applied in organic chemistry, instruments, measuring devices, etc., can solve problems such as complex structure and preparation process, and impurities that are not fully understood and valued

Active Publication Date: 2021-05-25
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, due to the complexity of its structure and preparation process, vincristine still has some easily produced impurities that have not been fully recognized and paid attention to. The research on the impurities of novel structures produced during the synthesis process of vincristine is a dynamic development and ongoing process

Method used

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  • A kind of vincristine compound impurity and its preparation method and application
  • A kind of vincristine compound impurity and its preparation method and application
  • A kind of vincristine compound impurity and its preparation method and application

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Effect test

Embodiment 1

[0046] A kind of its preparation method of vincristine compound impurity, comprises the following steps:

[0047] A. Preparation of crude vinblastine impurity product-I: Add 250 g of vinblastine total alkali sulfate, 3000 ml of acetone, 500 ml of acetic acid, and 1000 ml of acetic anhydride in a 30 L reaction tank, and stir. Add the mixed solution of 150ml of concentrated sulfuric acid, 200g of potassium dichromate and 15L of drinking water dropwise at -40°C. After the dropwise addition, the reaction was carried out for 1-2 hours, and the reaction of the raw material vinblastine was detected by TLC tracking (developing solvent, petroleum ether: chloroform: acetone: diethylamine=60:30:5:6). Stir slowly under an ice bath at -40°C, and slowly add 1500ml of concentrated ammonia water into the reaction tank dropwise. After mixing evenly, the pH of the solution is detected to be 8-9. 10L×5 trichloromethane extraction. The extracted chloroform solution was washed three times with 3...

Embodiment 2

[0053] A preparation method for vincristine compound impurities, comprising the following steps:

[0054] A. Preparation of crude vinblastine impurity product-I: Add 250 g of vinblastine total alkali sulfate, 2250 ml of acetone, 375 ml of acetic acid, and 750 ml of acetic anhydride in a 30 L reaction tank, and stir. A mixed solution of 125ml of concentrated sulfuric acid, 125g of potassium dichromate and 12.5L of drinking water was added dropwise at -42°C. After the dropwise addition, the reaction was carried out for 1-2 hours, and the reaction of the raw material vinblastine was detected by TLC tracking (developing solvent, petroleum ether: chloroform: acetone: diethylamine=60:30:5:6). Keep stirring slowly under the ice bath at -42°C, and slowly add 1500ml of concentrated ammonia water into the reaction tank dropwise. After mixing evenly, the pH of the solution is detected to be 8-9. 10L×5 trichloromethane extraction. The extracted chloroform solution was washed three times...

Embodiment 3

[0059] A preparation method for vincristine compound impurities, comprising the following steps:

[0060] A. Preparation of crude vinblastine impurity product-I: Add 750 g of vinblastine total alkali sulfate in a 100 L reaction tank, add 10.5 L of acetone, 1875 ml of acetic acid, and 4500 ml of acetic anhydride, and stir. Add the mixed solution of 600ml of concentrated sulfuric acid, 750g of potassium dichromate and 75L of drinking water dropwise at -45°C. After the dropwise addition, the reaction was carried out for 1-2 hours, and the reaction of the raw material vinblastine was detected by TLC tracking (developing solvent, petroleum ether: chloroform: acetone: diethylamine=60:30:5:6). Keep stirring slowly under the ice bath at -45°C, and slowly add 4500ml of concentrated ammonia water into the reaction tank dropwise. After mixing evenly, the pH of the solution is detected to be 8-9. 30L×5 trichloromethane extraction. The extracted chloroform solution was washed three times...

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Abstract

The invention relates to the technical field of medicinal chemistry, in particular to a vincristine compound impurity and its preparation method and application, comprising the following steps: adding acetone, acetic acid and acetic anhydride to vinca total alkaloid sulfate in proportion and then stirring; Slowly add the mixed solution of concentrated sulfuric acid, potassium dichromate and water that has been prepared dropwise, adjust to alkaline after the reaction is complete, and obtain the vincristine compound impurity after extraction, evaporation, concentration and purification, which is vincristine sulfate The quantitative and qualitative analysis of alkali impurity detection provides a reference or control.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a vincristine compound impurity and a preparation method and application thereof. Background technique [0002] Periwinkle (Catharanthus roseus) is an herbaceous plant of the family Apocynaceae, which is widely used in the folk to stop bleeding, relieve pain, clean wounds, and treat scurvy and diabetes. In the late 1950s, Noble et al. discovered vinblastine (VLB) and vincristine (VCR) with significant antitumor activity, and they have been used clinically so far. [0003] [0004] Vincristine drugs mainly act on the G1, S and M phases of the cell proliferation cycle, and have a delaying effect on the M phase, which can interfere with the formation of the spindle of proliferating cells, stop mitosis in the middle phase, and have immunosuppressive effects. specific antineoplastic drugs. "By inhibiting tubulin assembly, preventing the formation of the spindle, there...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D519/04G01N30/90
CPCC07D519/04G01N30/00G01N30/90G01N2030/009
Inventor 陈洪亮任翔袁诚黄建军易建峰潘振华李咏华王国财徐镇源许文东颜景胡
Owner GUANGZHOU HANFANG PHARMA
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