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Synthesis method of atropine and atropine sulfate

A technique for the synthesis of atropine sulfate, which is applied in organic chemistry and other fields, and can solve problems such as low reaction efficiency, uncertain quality of atropine, and difficulty in realizing commercial scale.

Pending Publication Date: 2020-06-09
合肥创新医药技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently known processes for the synthetic production of atropine or atropine sulphate suffer from a number of disadvantages that make their implementation difficult on a commercial scale
This is mainly due to the inefficiency of the reactions involved and the known methods require, for example, the isolation of intermediates, large excesses of reagents making the quality of the synthesized atropine uncertain

Method used

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  • Synthesis method of atropine and atropine sulfate
  • Synthesis method of atropine and atropine sulfate
  • Synthesis method of atropine and atropine sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A kind of synthetic method of atropine and atropine sulfate specifically comprises the steps:

[0044](1) Add 2.0kg (12.0mol) of tropic acid into the reactor, then add 6L of dichloromethane, form a suspension under stirring conditions, add DMF 0.088kg (1.2mol), then slowly add 1.235kg (12.0mol) of acetic anhydride dropwise for at least 30min, after the dropwise addition is completed, stir and react at 25°C for 3h to obtain a reaction solution that generates acetyltropic acid;

[0045] (2), add thionyl chloride 1.43kg (12.0mol) dropwise to the reaction solution that generates acetyltropic acid obtained in step (1), the dropwise addition time is at least 1h, after the dropwise addition is completed, stir the reaction at 25°C 2h, obtain the reaction solution that generates acetyl tropic acid chloride;

[0046] (3), 2.0kg (14.2mol) of tropinol was added to another reactor, then 6L of dichloromethane was added, after stirring to form a solution, the temperature was raised t...

Embodiment 2

[0051] A kind of synthetic method of atropine and atropine sulfate specifically comprises the steps:

[0052] (1) Add 2.0kg (12.0mol) of tropic acid into the reactor, then add 6L of dichloromethane, form a suspension under stirring conditions, add DMF 0.088kg (1.2mol), then slowly add acetyl chloride 1.13kg (14.4mol) dropwise, the dropwise addition time is at least 30min, after the dropwise addition is completed, stir and react at 25°C for 5h to obtain a reaction solution that generates acetyltropic acid;

[0053] (2), in the reaction solution that generates acetyltropic acid that step (1) obtains, dropwise add oxalyl chloride 1.84kg (14.5mol), the time for adding is at least 1h, after dropping, stir and react at 25°C for 2h, Obtain the reaction liquid that generates acetyl tropic acid chloride;

[0054] (3), 2.0kg (14.2mol) of tropinol was added to another reactor, then 6L of dichloromethane was added, after stirring to form a solution, the temperature was raised to 35°C, an...

Embodiment 3

[0059] A kind of synthetic method of atropine and atropine sulfate specifically comprises the steps:

[0060] (1) Add 2.0kg (12.0mol) of tropic acid into the reactor, then add 6L of toluene, form a suspension under stirring conditions, add 0.19% pyridine to the suspension at a stirring frequency of 40Hz and a temperature of 25°C kg (2.4mol), then slowly add acetyl chloride 0.94kg (12.0mol) dropwise, the dropwise addition time is at least 30min, after the dropwise addition is completed, stir and react at 25°C for 5h to obtain a reaction solution that generates acetyltropic acid;

[0061] (2), add phosphorus pentachloride 3.02kg (14.4mol) in the reaction solution that generates acetyltropic acid that step (1) obtains, after adding, stir reaction 4h at 35 ℃, obtain containing acetyltropic acid chloride The reaction solution;

[0062] (3), join 2.0kg (14.2mol) of tropinol in another reactor, then add 6L of toluene, stir to form a solution and then warm up to 35°C, add p-toluenesu...

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Abstract

The invention provides a synthesis method of atropine and atropine sulfate, which comprises the following steps: carrying out acetylation reaction on tropine acid to form acetyl tropine acid, reactingthe acetyl tropine acid with a chlorination reagent to form acyl chloride, reacting the acyl chloride with tropine alcohol, removing acetyl to obtain atropine, and salifying atropine and sulfuric acid to obtain atropine sulfate. The whole synthesis process can be completed by adopting a one-pot reaction, additional steps for completing the process by isolating intermediates are avoided, the reaction conditions are mild, the steps are simple, the yield is high, the purity is high, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation of pharmaceutical intermediates, in particular to a synthesis method of atropine and atropine sulfate. Background technique [0002] Atropine is a natural compound that is extracted from plants such as atropine belladonna, datura datura and dubuylan. Atropine competitively blocks the action of acetylcholine, a neurotransmitter, on the body's muscarinic receptors, which has been shown to dilate pupils, increase heart rate, and reduce salivation and other secretions. Atropine has many medicinal properties. More common usage includes administration before anesthesia to reduce mucous secretions such as saliva. During anesthesia and surgery, atropine is used to maintain a normal heart rate in some cases. Atropine sulfate, a salt of atropine, is also used to prevent or reverse the side effects of certain drugs and certain pesticides. Atropine is also used in ophthalmology. In this regard, atrop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 丁杨许龙曹阳黄美容
Owner 合肥创新医药技术有限公司
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