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Preparation method of norepinephrine bitartrate

A technology of norepinephrine and bitartrate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of cumbersome process, high preparation cost, poor reproducibility of synthesis route, etc., To achieve the effect of simple unit operation, improved reaction yield and controllable quality

Pending Publication Date: 2021-01-15
合肥亿帆生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiencies of the prior art, the present invention provides a method for preparing norepinephrine bitartrate, which solves the problem that the preparation process of norepinephrine bitartrate is cumbersome, the reproducibility of the synthetic route is poor, and the preparation high cost problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of norepinephrine bitartrate, comprising the following steps:

[0022] S1. Using chloroacetyl catechol as the starting material, conduct a coupling reaction with dibenzylamine in butanone solvent. After the reaction, add hydrochloric acid step by step to separate and purify the product. After the first drop of hydrochloric acid , dibenzylamine was precipitated as hydrochloride, and after the second dropwise addition of hydrochloric acid, 2-(benzhydrylamino)-3',4'dihydroxyacetophenone was precipitated as hydrochloride;

[0023] S2, 2-(benzhydrylamino)-3', 4'dihydroxyacetophenone hydrochloride is catalyzed by hydrogenation of 1% palladium carbon under 0.1MPa hydrogen pressure, and reduced in alcohol solvent to obtain exogenous racemic norepinephrine;

[0024] S3. Racemic norepinephrine is resolved by D-tartaric acid in aqueous alcohol solution to obtain L-norepinephrine D-tartrate. Before the separation, racemic norepinephrine and D-tartaric acid are...

Embodiment 2

[0028] A preparation method of norepinephrine bitartrate, comprising the following steps:

[0029] S1. Using chloroacetyl catechol as the starting material, conduct a coupling reaction with dibenzylamine in isopropanol solvent. After the reaction, add hydrochloric acid step by step to separate and purify the product. Add hydrochloric acid dropwise for the first time Finally, dibenzylamine was precipitated as hydrochloride, and after the second dropwise addition of hydrochloric acid, 2-(benzhydrylamino)-3',4'dihydroxyacetophenone was precipitated as hydrochloride;

[0030] S2, 2-(benzhydrylamino)-3',4'dihydroxyacetophenone hydrochloride is catalyzed by hydrogenation of 15% palladium carbon under 1MPa hydrogen pressure, and reduced in alcohol solvent to obtain racemic Norepinephrine;

[0031] S3. Racemic norepinephrine is resolved by D-tartaric acid in aqueous alcohol solution to obtain L-norepinephrine D-tartrate. Before the separation, racemic norepinephrine and D-tartaric ac...

Embodiment 3

[0035] A preparation method of norepinephrine bitartrate, comprising the following steps:

[0036] S1. Using chloroacetyl catechol as the starting material, conduct a coupling reaction with dibenzylamine in a mixed solvent of methyl ethyl ketone and isopropanol. After the reaction, add hydrochloric acid step by step to separate and purify the product. The first After the first drop of hydrochloric acid, dibenzylamine was precipitated as hydrochloride, and after the second drop of hydrochloric acid, 2-(benzhydrylamino)-3',4'dihydroxyacetophenone was precipitated as hydrochloride;

[0037] S2, 2-(benzhydrylamino)-3',4'dihydroxyacetophenone hydrochloride is catalyzed by hydrogenation of 20% palladium carbon under 2MPa hydrogen pressure, and then reduced in alcohol solvent to obtain racemic Norepinephrine;

[0038] S3. Racemic norepinephrine is resolved by D-tartaric acid in aqueous alcohol solution to obtain L-norepinephrine D-tartrate. Before the separation, racemic norepinephr...

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Abstract

The invention relates to the technical field of drug synthesis, and discloses a preparation method of norepinephrine bitartrate, which comprises the following steps of S1, taking chloroacetyl catecholas an initial raw material, carrying out a coupling reaction with dibenzylamine in a reaction solvent to obtain 2-(diphenylmethylamino)-3', 4' dihydroxyacetophenone hydrochloride, S2, carrying out hydrogenation catalysis on the 2-(diphenylmethylamino)-3', 4' dihydroxyacetophenone hydrochloride to reduce in the solvent to obtain racemic norepinephrine, S3, enabling racemic norepinephrine to be subjected to D-tartaric acid resolution in an alcohol-water solution, and acquiring L-norepinephrine D-tartrate, and S4, neutralizing the L-norepinephrine D-tartrate in water by alkali to obtain L-norepinephrine. Compared with the existing preparation method, the preparation method disclosed by the invention has the advantages that easily available starting materials are used, good reproducibility ofa synthetic route is ensured, unit operation is simple, economic accounting is realized, each step of reaction is easy to purify, the quality is controllable, and the reaction yield is greatly improved.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a preparation method of norepinephrine bitartrate. Background technique [0002] Drugs are substances used to prevent, treat and diagnose diseases. In theory, drugs refer to chemical substances that can affect the physiological functions of body organs and cell metabolism activities. With the rapid development of modern medicine, drugs There are many kinds of drugs, and norepinephrine bitartrate is one of them. It is mainly used for anti-shock, such as shock caused by anesthesia, toxic shock, cardiogenic shock, etc., but norepinephrine bitartrate is used in During the preparation, the process is relatively cumbersome, the reproducibility of the synthetic route is poor, and the preparation cost is relatively high. Contents of the invention [0003] (1) Solved technical problems [0004] Aiming at the deficiencies of the prior art, the present invention provides a method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/08C07C213/00C07C213/10C07C215/60
CPCC07C213/08C07C213/00C07C213/10C07C215/60
Inventor 钱莉苹黄凯黄勇吴世刚李刚
Owner 合肥亿帆生物制药有限公司
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