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Refining method for vincamine

A purification method and vincamine technology, applied in the direction of organic chemistry and the like, can solve the problems of difficult separation and removal, affecting the quality of vincamine, etc., and achieve the effects of easy operation, good removal effect and high safety.

Active Publication Date: 2017-05-31
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] This compound is similar to vincamine in structure and polarity, so it is difficult to separate and remove, which seriously affects the quality of vincamine

Method used

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  • Refining method for vincamine
  • Refining method for vincamine
  • Refining method for vincamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Step 1: Add 12.0g of vincamine crude product and 60ml of anhydrous organic solvent to a 100ml single-necked bottle. The selection of the organic solvent is shown in Table 1. Under stirring, the temperature is raised to 60°C for beating for 7 hours, then down to 25°C and stirred for 8 hours. Then lower it to 0°C for crystallization for 4 hours, filter with suction, wash the filter cake with 12 ml of cold methanol, and dry at 40°C for 6-9 hours. Obtain white vincamine beating product, N-oxide impurity, purity and yield situation are shown in Table 1.

[0034] Step 2: Add 6.0 g of vincamine slurry and 200 ml of dichloromethane into a 500 ml single-necked bottle, dissolve under stirring, filter, and concentrate the filtrate under reduced pressure to obtain a concentrate.

[0035]Step 3: Add the concentrate to a 250ml three-necked bottle, add 10ml of dichloromethane and 20ml of methanol, heat to 60°C for beating for 3 hours, lower to 21°C and stir for 7 hours, a large amount...

Embodiment 2

[0039] Step 1: Add 12.0g of crude vincamine and 60ml of N,N-dimethylformamide to a 100ml single-necked bottle, heat up to a certain temperature and beat for 7 hours while stirring. The selection of the temperature is shown in Table 2, and the temperature is lowered to 25°C Stir for 8 hours, then drop to 0°C to crystallize for 4 hours, filter with suction, wash the filter cake with 12ml of cold methanol, and dry at 40°C for 6-9 hours. Obtain white vincamine beating, N-oxide impurities, purity and yield are shown in Table 2.

[0040] Step 2: Add 6.0 g of vincamine slurry and 200 ml of dichloromethane into a 500 ml single-necked bottle, dissolve under stirring, filter, and concentrate the filtrate under reduced pressure to obtain a concentrate.

[0041] Step 3: Add the concentrate to a 250ml three-necked bottle, add 10ml of dichloromethane and 20ml of methanol, heat to 60°C for beating for 3 hours, lower to 21°C and stir for 7 hours, a large amount of white crystals are precipita...

Embodiment 3

[0045] Step 1: Add 12.0g of crude vincamine and 60ml of N,N-dimethylformamide to a 100ml single-necked bottle, raise the temperature to 60°C for 7 hours under stirring, lower the temperature to 25°C and stir for 8 hours, and then lower the temperature to 0°C for analysis After crystallization for 4 hours, filter with suction, wash the filter cake with 12ml of cold methanol, and dry at 40°C for 6-9 hours. 10.4 g of white vincamine slurry was obtained, with a molar yield of 87.0%.

[0046] Step 2: Add 6.0 g of vincamine slurry and 200 ml of organic solvent into a 500 ml single-necked bottle. The selection of the organic solvent is shown in Table 3. Dissolve under stirring, filter, and concentrate the filtrate under reduced pressure to obtain a concentrate.

[0047] Step 3: Add the concentrate to a 250ml three-neck bottle, add 10ml of dichloromethane and 20ml of methanol mixed solvent, heat to 60°C for beating for 3 hours, lower to 21°C and stir for 7 hours, filter with suction, ...

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Abstract

The invention relates to a refining method for vincamine and belongs to the field of refining of compounds. The method includes the following steps that 1, in existence of organic solvent, pulping is carried out on a vincamine rough product, then the vincamine rough product is cooled, crystallized and subjected to suction filtration, a filter cake is washed with the organic solvent, and a vincamine pulped product is obtained after drying; 2, the obtained vincamine pulped product is dissolved with the organic solvent and filtered, filtrate is subjected to vacuum concentration, and then concentrate is obtained; 3, organic solvent is added into the concentrate, the mixture is pulped, cooled, crystallized and subjected to suction filtration, a filter cake is washed with organic solvent, and a vincamine refined product is obtained after drying. The method has the advantages that the removal effect of N-oxide impurities is good, the reaction process is easy and convenient to implement, safety is high, cost is low, the yield of the obtained product is high, quality is good, and the vincamine is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for refining vincamine in the field of compound purification. Background technique [0002] Vincamine is one of the main alkaloids in Vinca minor, and it is the quinine class of monoterpene indole alkaloids. Its chemical name is (3α,14β,16α)-14,15-di Hydrogen-14-Dihydro-14-hydroxyeburnenine-14-carboxylic acid methylester, English chemical name (3a,14b,16a)-14,15-Dihydro-14-hydroxyeburnenine-14–carboxylicacid methylester, molecular formula: C 21 h 26 N 2 o 3 , molecular weight 354.4, the structural formula is as follows (formula Ⅰ): [0003] [0004] Vincamine can pass through the blood-brain barrier, maintain and restore the oxidative catabolism of glucose in the brain tissue of the diseased area, and restore the production of lactic acid and the release of carbon dioxide to normal, thereby dilating small cerebral blood vessels and improving cerebral circulation. The blood flow in the normal brain area of ​​the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D461/00
CPCC07D461/00
Inventor 张卫军李洋刘素娜白洁陶芳邸矾董爱军杨璐李冶韩晓丹王龙
Owner NORTHEAST PHARMA GRP
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