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Preparation method for atropine sulfate

A technology of atropine sulfate and hydrochloric acid, applied in the direction of organic chemistry, can solve the problems of incomplete racemization, cumbersome operation, and many impurities in the extraction, and achieve the effect of low cost, simple process operation, and less pollution

Active Publication Date: 2016-10-26
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned extraction methods have problems such as high solvent toxicity, many extraction impurities, and cumbersome operations. At the same time, the use of alkali-alcohol racemization also has problems such as incomplete racemization and cumbersome post-treatment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 5000g of daphnia japonica dry powder, add 4L of 1% hydrochloric acid to wet and expand, add it to the percolation bucket, add 1% hydrochloric acid to soak for more than 24 hours, then carry out percolation, control the percolation speed to flow out 2~3ml per minute, and collect the acid solution 5 L, extracted once with 2 L chloroform, adjusted the acid solution to pH~9 or above with ammonia water, extracted twice with 2 L×2 chloroform, combined the organic phases, dried over anhydrous sodium sulfate, and concentrated to dryness at 50~60°C in vacuo to obtain Brown-yellow thick paste 32.6 g.

[0015] Take 32.6 g of brown-yellow thick paste, dissolve it in 90 ml of acetone, add 1.50 g of activated carbon, heat and stir for half an hour to decolorize, filter, add 10% sulfuric acid dropwise to make it acidic, let it stand at room temperature, and then freeze it at 0~10°C overnight. The solid scopolamine sulfate was removed by filtration, and the filtrate was concentrat...

Embodiment 2

[0018] Take 5000g of datura dry powder, add 4L of 4% hydrochloric acid to wet and expand, add it to the percolation bucket, add 4% hydrochloric acid to soak for more than 24 hours, then carry out percolation, control the percolation speed to flow out 2~3ml per minute, and collect the acid solution 4.5 L, extracted once with 2 L chloroform, adjusted the acid solution to a pH above 9 with ammonia water, extracted twice with 2 L×2 chloroform, combined the organic phases, dried over anhydrous sodium sulfate, concentrated to dryness at 50~60°C in vacuo, 35.2 g of brown-yellow thick paste was obtained.

[0019] Take 35.2 g of brown-yellow thick paste, dissolve it in 90 ml of acetone, add 1.70 g of activated carbon, heat and stir for half an hour to decolorize, filter, add 10% sulfuric acid dropwise to make it acidic, let it stand at room temperature, and then freeze it at 0~10°C overnight. The solid scopolamine sulfate was removed by filtration, and the filtrate was concentrated to ...

Embodiment 3

[0022] Take 5000g of datura dry powder, add 4L of 2% hydrochloric acid to wet and expand, add it to the percolation bucket, add 2% hydrochloric acid to soak for more than 24 hours, then carry out percolation, control the percolation speed to flow out 2~3ml per minute, and collect the acid solution 5 L, extracted once with 2 L chloroform, adjusted the acid solution to pH~9 or above with ammonia water, extracted twice with 2 L×2 chloroform, combined the organic phases, dried over anhydrous sodium sulfate, and concentrated to dryness at 50~60°C in vacuo to obtain Brown yellow thick paste 33.2 g.

[0023] Take 33.2 g of brown-yellow thick paste, dissolve it in 90 ml of acetone, add 1.70 g of activated carbon, heat and stir for half an hour to decolorize, filter, add 10% sulfuric acid dropwise to make it acidic, let it stand at room temperature, and then freeze it at 0~10°C overnight. The solid scopolamine sulfate was removed by filtration, and the filtrate was concentrated in vacu...

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PUM

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Abstract

The invention discloses a preparation method for atropine sulfate. The preparation method comprises the following steps: 1) adding dry powder of daturae flower into hydrochloric acid with a concentration of 1 to 4% and a volume 0.5 to 1 time of the volume of the dry powder for wetting and swelling, then adding the swollen daturae flower powder into a percolating barrel, adding the hydrochloric acid with a concentration of 1 to 4%, dipping the powder for 24 h or above and carrying out percolating so as to obtain brown-yellow stiff paste; 2) dissolving brown-yellow stiff paste in acetone, adding active carbon, carrying out decoloring and filtering, adding acid drop by drop until a pH value is less than 7 and carrying out standing at room temperature so as to obtain hyoscyamine sulfate; and 3) spreading hyoscyamine sulfate on a sample disc, putting the sample disc into a baking oven, carrying out heating for racemization, then carrying out cooling to obtain a crude atropine sulfate product, adding ethanol, carrying out dissolving under stirring and then filtering, subjecting a filtrate to crystallization overnight and then successively carrying out pressure-reduced filtering and vacuum drying so as to obtain atropine sulfate. According to the invention, the daturae flower is used as a raw material; acid water is used for percolation and extraction; total alkali is obtained through chloroform extraction; sulfuric acid is added into an acetone solution for salt forming so as to obtain hyoscyamine sulfate, then heating is carried out for racemization, and ethanol recrystallization is carried out to obtain atropine sulfate; and the method is simple in process operation, small in pollution, low in cost and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of atropine sulfate, and belongs to the technical field of extraction and separation of traditional Chinese medicines and their synthesis and preparation. Background technique [0002] Atropine, i.e. racemic scopolamine, is extracted from plants belladonna and scopolamine, and can also be synthesized artificially. Its sulfate is a colorless or white crystalline powder, and it is an anticholinergic drug that blocks M-choline receptors. Relieve smooth muscle spasm (including relieving vasospasm and improving microvascular circulation); inhibit gland secretion; relieve the inhibition of vagus nerve on the heart and make the heart beat faster; dilate pupils and increase intraocular pressure; stimulate the respiratory center. [0003] The currently disclosed method for preparing atropine sulfate is divided into a synthesis method and an extraction method. Ye Songlin, Shen Jiaxiang. Compilation of national raw m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 王龙书傅玉萍肖乐扩蒋兆健卢嘉伟宋晓燕刘春芳李康强
Owner GUANGZHOU HANFANG PHARMA
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