Separation and purification method of oxidized camphor

A technology of separation and purification and camphor, which is applied in the field of chemical synthesis, can solve the problems that crystallization post-treatment methods cannot be removed, cannot meet the needs of separation, and the conditions of impurity synthesis are uncontrollable, etc., to solve the problems of insufficient selectivity, large sample loading, and easy The effect of industrial production

Active Publication Date: 2018-10-16
长春大政药业科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, camphor is used as raw material and produced by chemical synthesis methods, which may produce impurities such as monobromocamphor, dibromocamphor, hydroxycamphor, etc. The synthesis conditions of some impurities are uncontrollable, and post-treatment methods such as crystallization cannot be removed. Based on ordinary chromatographic separation methods and technologies has been unable to meet the needs of its separation

Method used

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  • Separation and purification method of oxidized camphor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1.5 g of crude oxidized camphor was dissolved in 7.5 mL of n-hexane-ethyl acetate, and the injection volume was 7.5 mL; a carboxyl silica gel column (column size 50×250 mm, particle size 10 microns, pore size 10 nm, packing mass 300 g) was used , column temperature 30 o C, flow rate 80mL / min; non-polar solvent is n-hexane, polar solvent is ethyl acetate, wherein the volume ratio of non-polar solvent / polar solvent is 90 / 10; ultraviolet detector, detection wavelength 280 nm, from the target Pick up fractions from the peak when the peak comes out and stop when the peak returns to the baseline. During the process of picking up fractions, pick up fractions every 3 minutes, and combine the fractions based on the results of liquid phase fraction analysis. After purification, the purity can be more than 98%, and the purity is less than 1%.

Embodiment 2

[0023] 0.3 g of crude oxidized camphor was dissolved in 2 mL of n-hexane-ethyl acetate solution, and the injection volume was 2 mL; a carboxyl silica gel column (column size 50×250 mm, particle size 10 microns, pore size 30 nm, packing mass 300 g ), column temperature 30 o C, flow rate 80 mL / min; non-polar solvent is n-hexane, polar solvent is ethyl acetate, wherein the volume ratio of non-polar solvent / polar solvent is 90 / 10; ultraviolet detector, detection wavelength 280 nm, from When the target peak comes out of the peak, pick up fractions until the peak returns to the baseline and stop. During the fraction pick-up process, pick up fractions every 3 minutes, and combine the fractions through the analysis results of liquid phase fractions. After purification, the purity can be more than 98%, and the purity is less than 1%. .

Embodiment 3

[0025] 10 g of crude oxidized camphor was dissolved in 50 mL of n-hexane-ethyl acetate solution, and the injection volume was 50 mL. A carboxyl silica gel column (column size 100×250 mm, particle size 10 microns, pore size 20 nm, packing mass 1.2 kg) was used, and the column temperature was 30 o C, flow rate 240 mL / min. The non-polar solvent is n-hexane, and the polar solvent is ethyl acetate, wherein the volume ratio of non-polar solvent / polar solvent is 90 / 10; the ultraviolet detector, the detection wavelength is 280 nm, and the fraction is connected from the target peak to the peak. The peak returns to the baseline and stops. During the fraction collection process, the fractions are collected every 3 minutes, and the fractions are combined through the analysis results of the liquid phase fractions. After purification, the purity can be more than 98%, and the purity is less than 1%.

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Abstract

An oxocamphor separation and purification method belongs to the technical field of chemical synthesis. The purpose of the invention is to provide an oxocamphor separation and purification method by using high efficiency preparation of a chromatography dynamic axial pressure column system (DAC column). The method includes the following steps: separating an oxocamphor crude product with a filtering membrane and using a DAC column for separation. The invention has the advantage of high selectivity. In view of the current oxocamphor purification problems, the invention provides the normal phase separation and purification method. The oxocamphor mixed components are separated in the chromatographic column, so as to effectively solve the problem of insufficient selectivity of a single hydrophobic interaction or ion exchange effect. The method also has the advantages of large carrying capacity, easiness for realization of industrial production, good repeatability, simple and controllable operation, easy realization of automation and stable process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis. Background technique [0002] π-oxidized camphor (I, the chemical name is 1,7-dimethyl-7-methoxybicyclo[2.2.1]-2-heptanone, or called: 8-oxidized camphor, p-oxidized camphor, etc.) Also known as Vita Rehabilitation, it is a stimulant for the respiratory and circulatory center and a cardiotonic drug. It is suitable for central dyspnea and circulatory failure, and can also be used for heart weakness and dyspnea in various diseases. It can enhance myocardial contractility and improve diastolic function, especially suitable for children with pneumonia and heart failure with diastolic and systolic insufficiency. The chemical structural formula of oxidized camphor: [0003] [0004] At present, camphor is used as raw material and produced by chemical synthesis method, which may produce impurities such as monobromocamphor, dibromocamphor, hydroxycamphor, etc. The synthesis conditions of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/79C07C49/523
CPCC07C45/79C07C49/523
Inventor 关大伟杜培革苑广信刘义国安利萍程媛姜锋周鹏悦马宝元张志阳郑娜史琳琳伦玉珊关恒
Owner 长春大政药业科技有限公司
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