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Synthesis method of atropine sulfate

A technology of atropine sulfate and atropine, which is applied in the direction of organic chemistry, can solve the problems of low reaction efficiency and difficulty in realizing commercial scale, and achieve the effect of improving product yield and stable quality

Active Publication Date: 2021-08-31
常州康普药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The current process for the synthesis of atropine sulfate suffers from a number of disadvantages that make it difficult to realize on a commercial scale, mainly due to the low efficiency of the reactions involved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] One, prepare tropin ester

[0034] (1), 31kg of toluene, 1kg of tropinol and 2.6kg of α-formylphenylacetic acid methyl ester were added to the reactor for stirring, and the temperature was raised to 110° C. for the reaction;

[0035] (2) After reacting for 3 hours, cool to 2° C. to crystallize for 8 hours, filter, and wash the filter cake with toluene twice until the washing solution is clear, filter and dry, and dry at 58° C. for 7 hours to obtain tropin ester with a yield of 96%.

[0036] 2. Preparation of atropine

[0037] (1) Add 2.8kg of methanol, 13.65kg of chloroform and 1kg of tropine ester into the reaction kettle, stir; control the temperature in the kettle below 15°C, add 188g of palladium carbon and 100g of glacial acetic acid in 3 times, and add within 1 hour Finished, then reacted at 12°C for 7h;

[0038] (2) After the reaction is completed, the palladium carbon is emptied and filtered out, and 3 times of drinking water is added, stirred for 10 minutes, ...

Embodiment 2

[0048] One, prepare tropin ester

[0049] (1), 31kg of toluene, 1kg of tropin alcohol and 2.6kg of α-formylphenylacetic acid methyl ester were added to the reactor for stirring, and the temperature was raised to 105° C. for the reaction;

[0050] (2) After reacting for 4 hours, it was cooled to 0° C. to crystallize for 8 hours, filtered, and the filter cake was washed twice with toluene until the washing solution was clarified, filtered, and dried at 58° C. for 7 hours to obtain tropin ester with a yield of 95.6%.

[0051] 2. Preparation of atropine

[0052] (1) Add 2.8kg of methanol, 13.65kg of chloroform and 1kg of tropine ester into the reaction kettle, stir; control the temperature in the kettle below 15°C, add 188g of palladium carbon and 100g of glacial acetic acid in 3 times, and add within 1 hour Finished, then reacted at 10°C for 8h;

[0053] (2) After the reaction is completed, the palladium carbon is emptied and filtered out, and 3 times of drinking water is added...

Embodiment 3

[0057] One, prepare tropin ester

[0058] (1), 31kg of toluene, 1kg of tropinol and 2.6kg of α-formylphenylacetic acid methyl ester were added to the reactor for stirring, and the temperature was raised to 110° C. for the reaction;

[0059] (2) After reacting for 3 hours, it was cooled to 5° C. to crystallize for 8 hours, filtered, and the filter cake was washed twice with toluene until the washing solution was clarified, filtered, and dried at 58° C. for 7 hours to obtain tropin ester with a yield of 95.8%.

[0060] 2. Preparation of atropine

[0061] (1) Add 2.8kg of methanol, 13.65kg of chloroform and 1kg of tropine ester into the reaction kettle, stir; control the temperature in the kettle below 15°C, add 188g of palladium carbon and 100g of glacial acetic acid in 3 times, and add within 1 hour Finished, then reacted at 15°C for 6h;

[0062](2) After the reaction is completed, the palladium carbon is emptied and filtered out, and 3 times of drinking water is added, stirr...

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PUM

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of atropine sulfate. The preparation method comprises the following steps: firstly preparing tropine ester, then preparing atropine, salifying to prepare atropine sulfate, and finally refining to obtain the product. In the preparation process of the tropine ester, the reaction temperature is strictly controlled to be 105-111 DEG C, and the crystallization temperature is controlled to be 0-5 DEG C, so that the yield of the tropine ester is improved. In the process of preparing atropine through reduction reaction, palladium-carbon is adopted as a catalyst, and the reaction temperature is strictly controlled to be 10-15 DEG C, so that the product quality is effectively improved. Sulfuric acid is diluted by preparing a sulfuric acid ethanol solution, and the dripping speed of the sulfuric acid ethanol solution is controlled, so that the stable quality of atropine sulfate is ensured.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method of atropine sulfate. Background technique [0002] Atropine is a natural compound, extracted from plants, that has many medicinal properties, including the ability to dilate the pupils, increase the heart rate, and reduce salivation and other secretions. More common usage includes administration before anesthesia to reduce mucus secretions. During anesthesia and surgery, atropine is used to maintain a normal heart rate in some cases. [0003] Atropine sulfate, chemical name α-hydroxymethylphenylacetyl tropinol sulfate monohydrate, is an anticholinergic drug, which can inhibit the secretion of glands and dilate pupils, and is mainly used for the treatment of smooth muscle spasm, gastric ulcer and twelve Intestinal ulcer disease, organophosphorus pesticide poisoning, septic shock, etc. [0004] The current process for synthesizing atropine sulfate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 殷晓伟王姝汤金春
Owner 常州康普药业有限公司
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