Preparation method for anticholinergic drug intermediate

An intermediate and anticholinergic technology, which is applied in the field of preparation of anticholinergic drug intermediates, can solve the problems of low reaction yield, long reaction time, and low yield, and achieve high yield, stable product quality, High safety effect

Pending Publication Date: 2018-12-21
XUCHANG HENGSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the synthetic methods reported in the literature take anhydrous citric acid as the starting raw material, react with oleum, the reaction time is long, and the reaction yield is low, and the yield is even lower when using monohydrate citric acid

Method used

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  • Preparation method for anticholinergic drug intermediate
  • Preparation method for anticholinergic drug intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 200g of concentrated sulfuric acid into the three-necked flask, stir and cool down to -5°C, take citric acid monohydrate (100.0g, 0.48mol), divide it into three parts, add one part to the concentrated sulfuric acid every 1 hour, and control the reaction at 0~ 30°C, react for 4 hours; take 50.0g of 4A molecular sieve and add to the reaction, continue to react for 4 hours; slowly pour the above reaction solution into 500.0g of ice-water mixture, control the temperature below 50°C , after dropping, cool down to 0°C to crystallize for 6 hours, filter with suction, and dry the filter cake at 60°C to obtain 55.4 g of acetonedicarboxylic acid. Yield 80.2%, purity 99.5%.

Embodiment 2

[0019] Add 500g of concentrated sulfuric acid into the three-necked flask, stir and cool down to -10°C, take citric acid monohydrate (100.0g, 0.48mol), divide it into three parts, add one part to the concentrated sulfuric acid every 1 hour, and control the reaction at 0~ 30°C, react for 8 hours; add 20.0g of phosphorus pentoxide into the reaction, and continue to react for 4 hours; slowly pour the above reaction solution into 800.0g of ice-water mixture, control the temperature at 50 Below 0°C, drop the temperature to 0°C to crystallize for 12 hours, filter with suction, and dry the filter cake at 60°C to obtain 60.9 g of acetonedicarboxylic acid. Yield 88.1%, purity 99.2%.

Embodiment 3

[0021] Add 300g of concentrated sulfuric acid into the three-necked flask, stir and cool down to -5°C, take citric acid monohydrate (100.0g, 0.48mol), divide it into three parts, add one part to the concentrated sulfuric acid every 1 hour, and control the reaction at 0~ 30°C, react for 2 hours; add 50.0g of phosphorus pentoxide into the reaction, and continue to react for 4 hours; slowly pour the above reaction solution into 800.0g of ice-water mixture, control the temperature at 50 Below 0°C, drop the temperature to 0°C to crystallize for 2 hours after dropping, filter with suction, and dry the filter cake at 60°C to obtain 64.0 g of acetonedicarboxylic acid. Yield 92.6%, purity 99.3%.

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Abstract

The invention discloses a preparation method for an anticholinergic drug intermediate. Acetone-dicarboxylic acid is a common intermediate for synthesizing medicines, and has a very high application value in organic synthesis. The preparation method comprises the following steps: using citric acid monohydrate as a starting raw material, using concentrated sulfuric acid as a dehydrating agent, and adding a suitable amount of a water absorbent. The method is capable of saving resources, and saving cost, stable in product quality and high in yield, and suitable for large-scale stable industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical drug synthesis, and in particular relates to a preparation method of an anticholinergic drug intermediate. Background technique [0002] Anticholinergic drugs have been used in clinical practice for a long time and there are various types. Commonly used ones include atropine, anisodamine, scopolamine, belladonna, antispasmodic spirit (scopolamine butylbromide), propensine, etc. This type of medicine can relax bronchial smooth muscle and gastrointestinal smooth muscle spasm to relieve asthma and gastrointestinal colic, and can also relieve colic and biliary colic caused by ureteral stones. Atropine rescue organophosphorus pesticide poisoning is indispensable. Rescue septic shock is also commonly used atropine or anisodamine. [0003] Anticholinergics have antisecretory and antispasmodic properties and are commonly used in gastrointestinal disorders. Chemical blockade of the vagus nerve, which i...

Claims

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Application Information

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IPC IPC(8): C07C51/373C07C59/185C07C303/24C07C305/06
CPCC07C51/373C07C303/24C07C59/185C07C305/06
Inventor 谷志勇蚩晓娜郭培
Owner XUCHANG HENGSHENG PHARMA
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