Method for preparing quinindium and cinchonine

A technology of quinidine and precipitation method, which is applied in the field of separation and purification, can solve the problems of low alkaloid content, low yield, and many working steps, and achieve the effect of simple and convenient economy and high yield

Inactive Publication Date: 2011-10-12
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the structures and physicochemical properties of quinine, quinidine, cinchonine, and cinchonidine, which are relatively high in cinchona alkaloids, have a high degree of closeness, although column chromatography separation is feasible, column chromatography The method has high technical requirements, many working steps, relatively long production cycle and generally low yield; the precipitation method of the second alkaloid salt is difficult to control in actual work due to the concentration of cinchona alkaloid solution and inorganic salt solution , it is often difficult to obtain a higher desired alkaloid salt precipitate or the content of alkaloid in the obtained alkaloid salt precipitate is not high, resulting in difficulties in separation and purification; in addition, due to the high volatility of ether, high safety requirements in use, The loss is very large, and the actual use effect of using ether as a solvent is poor, and it is difficult to obtain cinchonine with higher purity from the leached matter of ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of raw material A: mix cinchona bark (30-60 mesh powder) with toluene equivalent to 6 times the volume of cinchona bark, heat and reflux at 80-90°C for 4 times, then combine and concentrate to obtain The total alkaloid extract is dissolved in dilute sulfuric acid solution with a concentration of 10% by mass, so that the pH value of the solution is between 3 and 4. After filtering, the filtrate is heated to 60-70°C, and the concentration of 10% by mass is added under stirring. % sodium hydroxide to adjust the pH value of the solution to 6.5-7.0, after standing and cooling, the quinine sulfate precipitates out, and the solid matter of the quinine sulfate is filtered out. Then add sodium hydroxide solution with a concentration of 20% by mass to the filtrate to adjust the pH value of the solution to 10, place it, and separate out the total solids of the remaining cinchona alkaloids, filter the solids and dry at 60-70°C under normal pressure That is, raw mate...

Embodiment 2

[0034] (1) Preparation of raw material A: Mix cinchona bark (30-60 mesh powder) with 6 times the volume of toluene, heat and reflux at 80-90°C for 4 times, then combine and concentrate, and the obtained total alkaloid extract is used Dissolve the dilute sulfuric acid solution with a mass ratio concentration of 10%, so that the pH value of the solution is between 3 and 4. After filtering, heat the filtrate to 60~70°C, and add sodium hydroxide with a mass ratio concentration of 10% under stirring to adjust the solution. When the pH reaches 6.5-7.0, the quinine sulfate precipitates out after standing and cooling, and the solid quinine sulfate is filtered out. Then add sodium hydroxide solution with a mass ratio concentration of 20% to the filtrate to adjust the pH value of the solution to 10, place it, and separate out the total solids of the remaining cinchona alkaloids, filter the solids and dry them under normal pressure at 60 to 70°C. Starting material A is obtained.

[0035...

Embodiment 3

[0039] (1) Preparation of raw material A: soak cinchona bark (30-60 mesh powder) with 6 times the volume of toluene at 80-90°C for 4 times under reflux, then merge and concentrate, and the obtained total alkaloid extract can be obtained by mass ratio The concentration is 10% of the dilute sulfuric acid solution dissolved, so that the pH value of the solution is between 3 ~ 4, after filtration, the filtrate is heated to 60 ~ 70 ° C, and the pH of the solution is adjusted by adding sodium hydroxide with a mass ratio concentration of 10% under stirring. 6.5-7.0, quinine sulfate precipitates out after standing and cooling. Filter out the quinine sulfate solid matter, add the sodium hydroxide solution of mass ratio concentration 20% in the filtrate to adjust the pH value of solution to 10, place, separate out the total solid matter of remaining cinchona alkaloids, filter out the solid matter in The raw material A can be obtained by drying under normal pressure at 60-70°C.

[0040]...

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Abstract

The invention discloses a method for preparing quinindium and cinchonine. The method comprises the following steps: separating out quinine from a total alkaloid of Peruvian bark through a sulfate precipitation method so as to obtain a filtrate containing other alkaloids; basifying the filtrate until the pH value is not less than 10, collecting the obtained precipitate and drying the precipitate so as to obtain a raw material A; dissolving the raw material A with an organic solvent, filtering, separating an indissoluble substance from the filtrate; dissolving the indissoluble substance with a proper amount of alcohol solvent, adding activated carbon for decoloring, and then carrying out filtration and crystallization so as to obtain the cinchonine; and concentrating the filtrate until the volume of filtrate is 1 / 5-1 / 10 of the original volume, standing until a solid is separated out, dissolving the solid with a proper amount of alcohol solvent, adding the activated carbon for decoloring, and then carrying out filtration and crystallization so as to obtain the quinindium. The method is economical, simple and convenient and is in favor of amplification production; and the yield is high.

Description

technical field [0001] The invention particularly relates to a method for preparing quinidine and cinchonine, belonging to the field of separation and purification. Background technique [0002] Quinidine and cinchonine are alkaloids in cinchona bark except quinine. Quinidine is mainly used as anti-arrhythmia and other cardiovascular disease drugs; its derivatives such as dihydroquinidine and quinidine sulfate can be used as drugs and can also be used in chiral catalytic reactions. Cinchonine is an essential analytical reagent for the determination of tungsten ore by gravimetric analysis. Cinchonine and its derivatives are widely used in the preparation, separation and analysis of chiral drugs and chiral intermediates. [0003] The purification method of quinidine and cinchonine in the cinchona bark reported in the literature is usually after separating the quinine in the cinchona total alkaloids, and then separating and purifying other alkaloids to obtain quinidine and cin...

Claims

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Application Information

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IPC IPC(8): C07D453/04
Inventor 蒲含林姜华陈蓉蓉
Owner JINAN UNIVERSITY
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