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The preparation technology of semi-synthetic vincamine

A preparation process, the technology of vincamine, applied in the field of chemical drug synthesis process, can solve the problems of reducing the ratio of isomer formation, easy loss of activity, easy to burn, etc., and achieve the effect of reducing the amount of addition, reducing cost and reducing pressure

Inactive Publication Date: 2011-12-14
ZHANGJIAKOU GERUI HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] The purpose of this invention is to provide a kind of preparation technology of semi-synthetic method vincamine, to solve the extremely unstable hydrogenation catalyst of the prior art, be exposed to in the air and burn very easily, lose activity very easily and consumption is big; Hydrogenation reaction pressure High; unsafe preparation of monoperoxymaleic acid; reducing the ratio of isomers; purifying product quality to reach pharmaceutical grade standards

Method used

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  • The preparation technology of semi-synthetic vincamine
  • The preparation technology of semi-synthetic vincamine
  • The preparation technology of semi-synthetic vincamine

Examples

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Embodiment 1

[0047] 1. Preparation of Tabonine Hydrochloride:

[0048] In a 100L sealed enamel reactor, add 50Kg of industrial methanol, after starting the stirring, add 5Kg (13.42mol) of Tabonine hydrochloride, quickly add 1Kg (Tabonine hydrochloride quality 20 The mass percentage of pure Pd is 7% Pd / C (the manufacturer is Shaanxi Ruike New Materials Co., Ltd.), then the lid is sealed, replaced with 99.9% nitrogen for three times, and then hydrogen (purity ≥99.5 %) After replacing the hydrogen for three times, pass hydrogen to a pressure of 0.25Mpa, slowly increase the temperature to 25°C, and stir the reaction at a speed of 100r / min. After reacting for 10 hours, take a sample from the sampling hole and analyze with a TLC dot plate. The volume of the developing agent The ratio is ethyl acetate:petroleum ether=2:3, the amount is 5ml, under the ultraviolet lamp, observe with the wavelength of 254nm, until there is no raw material Tappening hydrochloride. After the reaction, the Pd / C is filter...

Embodiment 2

[0061] 1. Preparation of Tabonine Hydrochloride:

[0062] In a 100L stainless steel reactor, add 50Kg of industrial methanol, after starting the stirring, add 5Kg (13.42mol) of Tabonine hydrochloride, and quickly add 0.5Kg (Tabonine hydrochloride mass 10% ) Newly prepared 7% Pd / C, then add 1.5Kg wet weight in Example 1 to collect the sealed recovered Pd / C, seal the lid of the kettle, replace it with high-purity nitrogen three times, and then use hydrogen (purity ≥99.5% After replacing the hydrogen gas of) for three times, the pressure of hydrogen gas to the pressure gauge on the reactor is 0.35 Mpa, the temperature is slowly raised to 30℃, and the reaction is stirred. After 15 hours of reaction, samples are taken from the sampling hole and analyzed by TLC dot plate. The developing agent is acetic acid Ethyl: Petroleum ether = 2:3, under ultraviolet light, observe with a wavelength of 254nm, until there is no raw material Tabonine hydrochloride. After the reaction, filter Pd / C, w...

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Abstract

The invention relates to a synthetic process for chemical medicines, in particular to a process for preparing vincamine by a semisynthetic method. At present, the process for preparing the vincamine is divided into a total synthetic method and the semisynthetic method, wherein the semisynthetic method has the problems of unstable and inflammable hydrogenation catalyst, large using amount, high hydrogenation pressure, insecurity in the preparation of monoperoxide maleic acid and the like. The process comprises the following steps of: preparing tabersonine vincadifformine hydrochloride, preparing the monoperoxide maleic acid, performing oxidizing reaction, performing reduction reaction and transposition reaction, precipitating ammonia and purifying products, wherein the low-cost and stable Pd / C hydrogenation catalyst is selected to reduce the pressure of the hydrogenation reaction; tabersonine sulfate is replaced by the tabersonine hydrochloride; the monoperoxide maleic acid is preparedby using low-concentration hydrogen peroxide; the reaction temperature is below 0 DEG C, and security coefficients are improved; the temperature of the oxidizing reaction is reduced, and the generation of isomers is reduced; purification and solvent recrystallization are performed by column chromatography; and the quality of the products reaches the pharmaceutical-grade standard.

Description

Technical field [0001] The invention relates to a synthesis process of chemical drugs, in particular to a semi-synthetic method vinblastine preparation process. Background technique [0002] The English name of vincamine, CAS NO 1617-90-9, its chemical name is 14,15-dihydro-14β-hydroxy-(3α,16α)-ebumamenine-14-carboxylic acid methyl ester, and the molecular formula is C 21 H 26 N 2 O 3， The molecular weight is 354.43. White or light yellow crystalline powder, insoluble in water, slightly soluble in alcohols, soluble in chloroform or dichloromethane, melting point 229℃-231℃, [α] D 25 +39 。 To +43 。 (C=0.0282, pyridine), IR: λcm -1 :1756,1074,747,727; UV has maximum absorption at 220nm and 268nm, and minimum absorption at 243nm. [0003] Vinblastine can penetrate the blood-brain barrier to maintain and restore the oxidative catabolism of glucose in the brain tissue of the diseased area, restore the production of lactic acid and the release of carbon dioxide to normal, thereby dilate s...

Claims

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Application Information

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IPC IPC(8): C07D461/00
Inventor 孙文王毅卢鹏李君杨国辉李世江
Owner ZHANGJIAKOU GERUI HIGH TECH
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