Method for synthesizing doxylamine succinate through base catalysis

A technique for the synthesis of doxylamine succinate and its synthesis method, which is applied in the field of raw material drug synthesis, and can solve the problems of sodium amide being dangerous, not easy to store, and the price of 2-chloroethyldimethylamine is expensive.

Pending Publication Date: 2022-05-24
GUANGXI BOTANICAL GARDEN OF MEDICINAL PLANTS
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  • Abstract
  • Description
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Problems solved by technology

[0011] In this route, the raw material 2-chloroethyl dimethylamine in the third step is expensive and difficult to store, and a large amount of sodium amide is dangerous to use and difficult to operate in large-scale production

Method used

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  • Method for synthesizing doxylamine succinate through base catalysis
  • Method for synthesizing doxylamine succinate through base catalysis
  • Method for synthesizing doxylamine succinate through base catalysis

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Embodiment Construction

[0031] Synthesis of 1, 2-pyridylphenyl methyl methanol

[0032]Weigh 34.2g (1.42mol) magnesium chips and 50mg (0.20mmol) iodine into a 2L four-mouth bottle, add 1.2L anhydrous tetrahydrofuran, nitrogen protection, the reaction solution is heated to reflux. Weigh 195.6 g (1.24 mol) bromobenzene mixed with 195 g of tetrahydrofuran, slowly added to the reaction solution. About two hours in drops. After the reaction is initiated, the tetrahydrofuran is refluxed in large quantities, and the reaction liquid becomes turbid and the color gradually becomes metallic gray. Keep the tetrahydrofuran backflow for two hours. Weigh 100 g (0.83 mol) 2-acetylpyridine mixed with 100 g of tetrahydrofuran, slowly added to the above Grigald reagent, about three and a half hours. The mixture is immediately produced by the white milk when the mixture is dripped into the Grignard reagent, and a large amount of exothermic, anhydrous tetrahydrofuran reflux. After the drop-added, the solution becomes clear, ...

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Abstract

The invention relates to a synthesis method of doxylamine succinate, which takes 2-acetylpyridine as an initial raw material, comprises the following unit processes: synthesis of doxylamine, salt forming reaction of doxylamine, separation and purification of doxylamine, and is characterized in that the synthesis of doxylamine comprises the following steps: firstly, reacting 2-acetylpyridine with a Grignard reagent generated by bromobenzene and magnesium to generate 2-pyridyl phenyl methyl methanol; then reacting 2-pyridyl phenyl methyl methanol with 2-chloroethyl dimethylamine hydrochloride under the catalysis of potassium tert-butoxide (or other alkane alkoxide potassium or sodium salt or potassium hydroxide or sodium hydroxide) to generate doxylamine; and finally salifying doxylamine and succinic acid to obtain the target product doxylamine succinate.

Description

Technical field [0001] The present invention relates to the field of API synthesis technology, specifically a method of synthesizing doxylamine succinate. Background [0002] Doxylamine succinate is an ethanolamine antihistamine, which has antihistamine effect, anticholinergic effect and sedative effect, suitable for a variety of allergic skin diseases, allergic rhinitis, asthmatic bronchitis, etc.; can also be used as a hypnotic for short-term treatment of insomnia. The overall reaction rate is high and the tolerance is good. At present, the synthesis process of doxylamine succinate has the following methods: [0003] 1. Synthesis of the key intermediate α-methyl-α-phenylpyridine-2-methanol under the catalysis of butyl lithium and benzophenone was used as raw material to prepare doxylamine: [0004] [0005] The first step of the reaction of the route to use n-butyl lithium, this substance in contact with water spontaneous combustion, very flammable, in large-scale production ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/30C07C51/41C07C55/10
CPCC07D213/30C07C51/412C07C55/10Y02P20/584
Inventor 刘凤鸣曲韵智师凤华谭木秀
Owner GUANGXI BOTANICAL GARDEN OF MEDICINAL PLANTS
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