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Method for converting natural deacetylated lappaconitine into lappaconitine

A technology of high clathrin and deacetylation, applied in directions such as organic chemistry, can solve problems such as high production cost, low product yield, product waste, etc., and achieve the effects of high utilization rate, reduced production cost, and less waste

Inactive Publication Date: 2013-09-11
XIAN RAINBOW BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product yield of this method is very low, resulting in great waste of products, complicated and time-consuming procedures, resulting in high production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 5.0 kg of alumina to a glass chromatography column with a specification of 100*1500 to make an adsorption column for use.

[0049] Get the crude product of raw material 2208g homogenate, dissolve in 10L chloroform. Then the obtained solution was added to an adsorption column, the filtrate was collected, and the content of N-deacetylhokinine in the filtrate was detected by HPLC. Through detection and calculation, the content of N-deacetylhomoquinone is 247g.

[0050] Then the collected filtrate was transferred to a 20L glass reaction kettle, 5.27g of DMAP was added, stirred and dissolved, and then 128ml of triethylamine was added, stirred and mixed.

[0051] Turn on the heating switch to heat the temperature of the reactor to 50°C.

[0052] Measure 39.8ml of acetyl chloride into the constant pressure dropping funnel, dilute to 240ml with chloroform, add dropwise at a rate of 2.4ml / min, after the dropwise addition, continue to react for 30min, extract with 1.1% dilu...

Embodiment 2

[0054] Add 4.8 kg of alumina to a glass chromatography column with a specification of 100*1500 to make an adsorption column for use.

[0055] Get the crude product of raw material 2146g homogenate, dissolve in 9.5L chloroform. Then the obtained solution was added to an adsorption column, the filtrate was collected, and the content of N-deacetylhokinine in the filtrate was detected by HPLC. Through detection and calculation, the content of N-deacetylhomoquinone is 296g.

[0056] Then the collected filtrate was transferred to a 20L glass reaction kettle, 5.27g of DMAP was added, stirred and dissolved, and then 128ml of triethylamine was added, stirred and mixed.

[0057] Turn on the heating switch to heat the temperature of the reactor to 52°C.

[0058] Measure 47.7ml of acetyl chloride into the constant pressure dropping funnel, dilute to 286ml with chloroform, add dropwise at a rate of 2.6ml / min, after the dropwise addition, continue to react for 30min, extract with 1.1% dilut...

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Abstract

The invention belongs to the field of natural drug extraction and concretely relates to a method for converting natural deacetylated lappaconitine into lappaconitine. The method comprises the following steps of: adding raw materials into an organic solvent, stirring to dissolve the raw materials, wherein the raw materials contain N-deacetylated lappaconitine; adding 4-dimethylaminopyridine and triethylamine, stirring and mixing; and heating the mixture to 45-60 DEG C, dropwise adding an acetylation reagent, and reacting for 0.3-1h after the dropwise adding operation is finished. By using the method disclosed by the invention, the yield of the lappaconitine can be greatly increased, the utilization ratio is high, and the waste is reduced; in addition, the process is simple and feasible, and the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the field of extraction of natural medicines, and in particular relates to a method for converting natural deacetylated homogenin into homogenin. Background technique [0002] Lappaconitine is a natural alkaloid extracted from the roots of Aconitum and other plants, the English name is Lappaconitine, and the molecular formula is C 32 h 44 N 2 o 8 , molecular weight 584.64, CAS accession number 32854-75-4. [0003] Gaowujiasu has a strong analgesic effect, the analgesic effect is equivalent to that of pethidine, 7 times that of the common analgesic drug aminopyrine, and the analgesic effect lasts longer. The anesthetic isomer of Gaoaconitum has a strong anesthetic effect from deep to superficial, and it has been clinically proven that the local anesthetic effect is equivalent to that of cocaine; the nerve conduction block effect is 5.25 times that of cocaine and 13 times that of procaine; Infiltration anesthesia is much str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
Inventor 赵彩红崔浪军桂计成
Owner XIAN RAINBOW BIO TECH CO LTD
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