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Vinpocetine compound and its preparation method

A technology of vinpocetine and its preparation method, which is applied in the field of compound and its preparation method, and the field of preparation method of vinpocetine compound, which can solve the problems of no public purification method, etc., and achieve the effects of reducing toxic and side effects, convenient operation, and mild reaction conditions

Inactive Publication Date: 2015-05-27
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The prior art does not disclose a dedicated purification method, so it is necessary to further purify the unqualified products to provide high-purity compounds in high yields

Method used

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  • Vinpocetine compound and its preparation method
  • Vinpocetine compound and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation of embodiment 1 Vinpocetine

[0037] (1) 10g vinpocetine crude product (purity 98.63%) is dissolved in 50ml dichloromethane, then add 10g neutral aluminum oxide and stir evenly, add to the chromatographic column upper end prepared after waving off solvent, wherein the filler of column is ICN allumina N neutral alumina with a particle size of 18-32 μm and a pore size of 6 nm, a column length of 40 cm, a diameter of 4 cm, and a column pressure of 0.5 Pa, and then pumped into a mixed solvent of ethyl acetate and isopropanol with a volume ratio of 75:25 for column Chromatography, the flow rate is 0.6ml / min, the column temperature is room temperature, start timing, take samples, track and monitor, collect in sections, and collect the eluted parts of vinpocetine;

[0038] (2) The above-mentioned vinpocetine eluent part was evaporated to dryness under reduced pressure, 100ml of isopropanol was added, heated to reflux for 10 minutes, cooled to 0°C overnight, the...

Embodiment 2

[0042] The preparation of embodiment 2 Vinpocetine

[0043] (1) 15g vinpocetine crude product (purity 98.77%) is dissolved in 60ml dichloromethane, then add 15g neutral aluminum oxide and stir evenly, add to the chromatographic column upper end prepared after waving off solvent, wherein the filler of column is Baker column chromatography special neutral alumina with a particle size of 50-200 μm and a pore size of 6 nm, with a column length of 40 cm, a diameter of 4 cm, and a column pressure of 1.5 Pa, and then pump a mixed solvent of ethyl acetate and isopropanol with a volume ratio of 75:25 Carry out column chromatography, the flow rate is 2.0ml / min, the column temperature is room temperature, start timing, take samples, track and monitor, collect in sections, and collect the eluted parts of vinpocetine;

[0044] (2) The above-mentioned vinpocetine eluent part was evaporated to dryness under reduced pressure, 100ml of isopropanol was added, refluxed for 30 minutes, cooled to ...

Embodiment 3

[0048] The preparation of embodiment 3 Vinpocetine

[0049] (1) 14g vinpocetine crude product (purity 98.56%) is dissolved in 55ml dichloromethane, then add 14g neutral aluminum oxide and stir evenly, add to the chromatographic column upper end prepared after waving off solvent, wherein the filler of column is ICN allumina N neutral alumina with a particle size of 18-32 μm and a pore size of 6 nm, a column length of 40 cm, a diameter of 4 cm, and a column pressure of 1.0 Pa, and then pumped into a mixed solvent of ethyl acetate and isopropanol with a volume ratio of 75:25 for column For chromatography, the flow rate is 1.0ml / min, the column temperature is room temperature, start timing, take samples, track and monitor, collect in sections, and collect the eluted parts of vinpocetine;

[0050] (2) The above-mentioned vinpocetine eluent part was evaporated to dryness under reduced pressure, 100ml of isopropanol was added, heated to reflux for 20 minutes, cooled to 4°C overnight,...

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Abstract

The invention discloses a vinpocetine compound and its preparation method. The method comprises the steps of: dissolving a vinpocetine crude product with a proper amount of an organic solvent, then carrying out column chromatography sample loading, taking neutral alumina as a stationary phase, using a mixed solvent of ethyl acetate and isopropyl alcohol as a mobile phase, performing elution under a column temperature of room temperature, then collecting the eluent; and subjecting a vinpocetine eluent part to pressure reduced evaporation to dryness, carrying out recrystallization with isopropyl alcohol, and performing drying, thus obtain the vinpocetine. With the advantages of simple process, low cost and high yield, the method provided in the invention improves the product quality of the preparation, reduces toxic and side effects, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a compound and a preparation method thereof, in particular to a preparation method of a vinpocetine compound, which belongs to the technical field of medicines. Background technique [0002] Vinpocetine (Calan), also known as apovincine ethyl ester, white or off-white crystalline powder, chemical name: (3α, 16α)-ivory phenin-14-carboxylic acid ethyl ester, molecular formula: C 22 h 20 N 2 o 2 , molecular weight: 350.45, structural formula: [0003] [0004] Vinpocetine was first developed by Gedeon Richter Company in Hungary and launched in 1978. Its pharmacological effects include: (1) increase cerebral blood flow; (2) promote the uptake and utilization of glucose and oxygen in the brain, increase ATP, and reduce the production of lactic acid during ischemia and hypoxia; (3) prevent brain cell excitotoxic death (excessive receptor excitation caused by excitatory amino acids); (4) reduce cerebral hypoxia damage and pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D461/00A61K31/4375A61P25/28
Inventor 陶灵刚
Owner HAINAN LINGKANG PHARMA CO LTD