Preparation method of doxylamine succinate impurity C

A technique for doxylamine succinate and impurities, which is applied in the field of preparation of doxylamine succinate impurity C, can solve the problems that doxylamine impurities have not been reported in the literature, and achieve high product yield, high purity, The effect of mild reaction conditions

Inactive Publication Date: 2017-11-24
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

However, there are very few reports on the synthesis of doxylamine impurities at home and abroad, especially the synthesis of doxylamine impurity C has not yet been reported in the literature.

Method used

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  • Preparation method of doxylamine succinate impurity C
  • Preparation method of doxylamine succinate impurity C
  • Preparation method of doxylamine succinate impurity C

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]

[0035] A kind of preparation method of doxylamine succinate impurity C that the present invention proposes, comprises the following steps:

[0036] 1. Treatment of 2-dimethylaminochloroethane hydrochloride

[0037] Weigh 5.0g of 2-dimethylaminochloroethane hydrochloride (34.6mmol) and dissolve it in 20mL of purified water, stir to dissolve, add 20mL of xylene, stir, cool to 0-5°C, add potassium hydroxide solution (hydrogen Potassium oxide (2.7g, purified water 10mL) solution, stirred for 30min, allowed to stand for stratification, collected the organic layer, continued to extract the water layer once with 20mL xylene, combined the organic layer, added anhydrous sodium sulfate and stirred vigorously for 20min, filtered to obtain 2 -Xylene solution of dimethylaminochloroethane, for subsequent use.

[0038] 2. Preparation of doxylamine succinate impurity C:

[0039] Add 6.4g of α-phenyl 2-pyridylmethanol (34.6mmol) and 50mL of toluene into the reactor, stir and diss...

Embodiment 2

[0041]

[0042] A kind of preparation method of doxylamine succinate impurity C that the present invention proposes, comprises the following steps:

[0043] 1. Treatment of 2-dimethylaminochloroethane hydrochloride

[0044] Weigh 6.0g of 2-dimethylaminochloroethane hydrochloride (41.7mmol) and dissolve it in 30mL of purified water, stir to dissolve, add 30mL of xylene, stir, cool to 0-5°C, add potassium hydroxide solution (hydrogen Potassium oxide 3.0g, purified water 10mL) solution, stirred for 30min, allowed to stand for stratification, collected the organic layer, continued to extract the water layer once with 20mL xylene, combined the organic layer, added anhydrous sodium sulfate and stirred vigorously for 25min, filtered to obtain 2 -Xylene solution of dimethylaminochloroethane, for subsequent use.

[0045] 2. Preparation of doxylamine succinate impurity C:

[0046] Add 6.4g of α-phenyl 2-pyridylmethanol (34.6mmol) and 60mL of toluene into the reactor, stir and disso...

Embodiment 3

[0048]

[0049] A kind of preparation method of doxylamine succinate impurity C that the present invention proposes, comprises the following steps:

[0050] 1. Treatment of 2-dimethylaminochloroethane hydrochloride

[0051] Weigh 7.0g of 2-dimethylaminochloroethane hydrochloride (48.6mmol) and dissolve it in 20mL of purified water, stir to dissolve, add 20mL of xylene, stir, cool to 0-5°C, add potassium hydroxide solution (hydrogen Potassium oxide (3.2g, purified water 10mL) solution, stirred for 30min, allowed to stand for stratification, collected the organic layer, continued to extract the water layer once with 20mL xylene, combined the organic layer, added anhydrous sodium sulfate and stirred vigorously for 30min, filtered to obtain 2 -Xylene solution of dimethylaminochloroethane, for subsequent use.

[0052] 2. Preparation of doxylamine succinate impurity C:

[0053] Add 6.4g of α-phenyl 2-pyridylmethanol (34.6mmol) and 60mL of toluene into the reactor, stir and dissol...

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Abstract

The invention discloses a preparation method of a doxylamine succinate impurity C. The preparation method comprises steps as follows: alpha-phenyl-2-pyridinemethanol and an organic solvent are added to a reactor, stirred and dissolved, after air in the reactor is subjected to N2 replacement, alkali liquor is added, a 2-dimethylaminoethyl chloride solution is dropwise added during stirring, a mixed solution is heated to produce backflow and is cooled after the reaction, water is added to a reaction product, a mixture is layered and purified, and a target product is obtained. According to the preparation method, alpha-phenyl-2-pyridinemethanol is taken as a raw material and subjected to an elimination reaction with 2-dimethylaminoethyl chloride under the alkaline condition, and the target product is obtained; the method has the advantages of adopting mild reaction conditions and short synthesis route and being simple and convenient to operate and can be applied to qualitative and quantitative analysis of impurities in doxylamine succinate production, and therefore, quality standard of doxylamine succinate can be improved; the product is high in yield and purity.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a method for preparing doxylamine succinate impurity C. Background technique [0002] Doxylamine succinate, chemical name: N,N-dimethyl-2-[1-phenyl-1-(2-pyridine)ethoxy]ethylamine succinate, CAS: 562 -10-7. Doxylamine succinate is a kind of ethanolamine drug, which has antihistamine effect, anticholinergic effect and significant sedative effect. It has strong activity and low gastrointestinal side effects, and is suitable for a variety of allergic skin diseases. Hay fever, allergic rhinitis, asthmatic bronchitis, etc. In October 1978, the FDA approved the marketing of doxylamine 25mg tablets of CHATTEM, which was used to help alleviate difficulty in falling asleep. It became OTC in 1979, approved in September 1996 and approved the listing of generic drugs of LNK in August 2004. On April 8, 2013, the FDA approved Diclegis (doxylamine succinate and pyridox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/30
CPCC07D213/30
Inventor 曹明成刘宏亮年帅
Owner 合肥创新医药技术有限公司
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