Method for preparing quinindium and cinchonine

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...

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