New process for preparing cytisine

A technology of cytisine and a new process, which is applied in the field of preparation of cytisine, can solve the problems of large loss and consumption, difficult handling of solvents, etc., and achieve the effects of less loss, high yield and simple steps

Inactive Publication Date: 2017-10-20
王答祺
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires column chromatography, the loss and consumption are large, and a part of the solvent adsorbed on the column is not easy to handle

Method used

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  • New process for preparing cytisine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1, a kind of new technique for preparing cytisine, such as figure 1 shown, including the following steps

[0015] ① Grinding the raw material, edamame grass, soaking and extracting with ethanol, filtering and combining the filtrates, and concentrating the filtrates to obtain extracts.

[0016] ②Primary extraction: Transfer the extract to an extraction tank, adjust the pH to <4 with sulfuric acid, add chloroform to the extraction tank, and stir for extraction. The chloroform layer was separated, and the same method was operated three times, the water layer was collected, and the chloroform was recovered.

[0017] ③Secondary extraction: the water layer extract was adjusted to pH > 10 with sodium hydroxide solution to free cytisine, and then extracted with chloroform until the water layer had no alkaloid reaction, and the water layer was discarded.

[0018] ④ Concentrating the chloroform layer to obtain the total alkaloids, dissolving them in acetone, cooling,...

Embodiment 2

[0021] Embodiment 2, a kind of new process for preparing cytisine, comprises the following steps

[0022] ①Take 500kg of crushed herb and 6000L of 85% ethanol and soak for 24 hours. They were extracted three times at a temperature of 80° C., and the combined filtrates were filtered. The filtrate was recovered under the condition of temperature 80°C and vacuum degree of -0.050~-0.070MPa to obtain 200kg of extract.

[0023] ②Primary extraction: add the extract to the extraction tank, and adjust the pH to <4 with sulfuric acid. Add chloroform to extract at a ratio of 3:1 between chloroform and extract for 2-3 times to remove all organic impurities, separate the chloroform layer and recover chloroform at a temperature of 80°C.

[0024] ③Secondary extraction: the aqueous layer was adjusted to pH>10 with sodium hydroxide solution to free cytisine, and then extracted with chloroform until the aqueous layer had no alkaloid reaction, and the aqueous layer was discarded.

[0025] ④ C...

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Abstract

The invention discloses a new process for preparing cytisine. The process comprises the steps of crushing a raw material, i.e., Thermopsis lanceolate grass, then, carrying out soaking extraction by 85% ethanol, carrying out filtrating, concentrating the filtrate to obtain an extract, subjecting the extract to double extraction to obtain a concentrate chloroform layer, concentrating the chloroform layer to obtain total alkaloids, carrying out dissolving by using acetone, carrying out crystallization to obtain crude cytisine crystals, dissolving the crude cytisine crystals with ethyl acetate, carrying out cooling recrystallization, carrying out dissolving by using acetone, carrying out cooling recrystallization, carrying out filtrating, carrying out vacuum drying, carrying out crushing, and then, carrying out screening and uniform mixing, thereby finally obtaining finished cytisine. According to the new process, the steps are simple, the operation is convenient, the crystallization rate is high, standing is not required, column chromatography is not required, the loss is low, the yield is high, and the obtained product is high in purity.

Description

technical field [0001] The invention relates to a preparation method of cytisine. Background technique [0002] As a raw material of smoking cessation preparation with obvious curative effect, cytisine has attracted the attention of the international medical community, and it is extracted from the phyllo plant. Cytisine has a similar effect on the respiratory system as nicotine, and can reflexively excite breathing. The excitatory effect is stronger than that of lobeline at the same dose. Its smoking cessation effect is certain and the price is low. [0003] The authorized publication number is CN101891740A, and the publication date is November 24, 2010. The title of the invention is "A Method for Extracting Cytisine from the Aerial Parts of Coniferae Huanghua Grass", and the method for extracting cytisine is disclosed as, The aboveground part of the lanceolate Huanghua grass is crushed, extracted and concentrated to obtain the extract. Acidifying the extract to obtain an ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/18
CPCC07D471/18
Inventor 王答祺
Owner 王答祺
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