Preparation method for amifostine

A technology of amifostine and aminopropylamino, which is applied in the field of drug preparation, can solve the problems of low yield, long reaction time, and difficult control, and achieve the effects of high yield, short reaction time, and easy control

Active Publication Date: 2013-06-12
KAIFENG MINGREN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide an improved amifostine preparation method aimed at the shortcomings of the existing amifostine synthesis process, such as low yield, long reaction time, and difficult control.

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  • Preparation method for amifostine
  • Preparation method for amifostine

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The preparation method of amifostine of the present invention, the detailed steps of this preparation method are as follows:

[0035]a. Preparation of ammonium salt: First, put the basic raw material N-(2-hydroxyethyl)-1,3-propylenediamine into the reaction vessel, and add concentrated hydrochloric acid (mass percent of concentrated hydrochloric acid) dropwise under constant stirring. The concentration is 36%), the molar ratio between N-(2-hydroxyethyl)-1,3-propanediamine and concentrated hydrochloric acid is 1:2, after the concentrated hydrochloric acid is added dropwise, at 40°C Under the conditions of reaction for 60 minutes, after the reaction, the reaction solution was concentrated to dryness, and after concentration, crystallization was carried out with ethanol (the amount of ethanol added was 8 times the weight of the concentrated product), and after crystallization, it was dried (in an oven carry out drying, the drying temperature is 50°C, and the drying time is...

Embodiment 2

[0042] The preparation method of amifostine of the present invention, the detailed steps of this preparation method are as follows:

[0043] a. Preparation of ammonium salt: First, put the basic raw material N-(2-hydroxyethyl)-1,3-propylenediamine into the reaction vessel, and add concentrated hydrochloric acid (mass percent of concentrated hydrochloric acid) dropwise under constant stirring. The concentration is 38%), the molar ratio between N-(2-hydroxyethyl)-1,3-propanediamine and concentrated hydrochloric acid is 1:1.8, after the concentrated hydrochloric acid is added dropwise, at 60°C After the reaction, the reaction solution was concentrated to dryness, and then crystallized with ethanol (the amount of ethanol added was 6 times the weight of the concentrated product), and dried after crystallization (in an oven carry out drying, the drying temperature is 40°C, and the drying time is 8h), and N-(2-hydroxyethyl)-1,3-propanediamine hydrochloride is obtained after drying; ...

Embodiment 3

[0050] The preparation method of amifostine of the present invention, the detailed steps of this preparation method are as follows:

[0051] a. Preparation of ammonium salt: First, put the basic raw material N-(2-hydroxyethyl)-1,3-propylenediamine into the reaction vessel, and add concentrated hydrochloric acid (mass percent of concentrated hydrochloric acid) dropwise under constant stirring. The concentration is 36%), the molar ratio between N-(2-hydroxyethyl)-1,3-propylenediamine and concentrated hydrochloric acid is 1:2.5, after the concentrated hydrochloric acid is added dropwise, at 30°C Under the conditions of reaction for 60min, after the reaction, the reaction solution was concentrated to dryness, and after concentration, crystallization was carried out with ethanol (the amount of ethanol added was 9 times the weight of the product obtained after concentration), and after crystallization, it was dried (in an oven carry out drying, the drying temperature is 60°C, and th...

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Abstract

The invention discloses a preparation method for amifostine. The preparation method comprises the following steps of: adding concentrated hydrochloric acid dropwise into N-(2-hydroxylethyl)1,3propane diamine serving as a basic raw material and reacting; after the reaction is finished, concentrating, devitrifying and drying to obtain ammonium salt; reacting the obtained ammonium salt with a chlorating agent and a catalyst; after the reaction is finished, performing treatment to obtain chloride, namely 2-(3aminopropyl amino)ethyl dichlorohydrochloride; adding sulfo-sodium phosphate and purifiedwater into a reaction vessel; adding potassium iodide and stirring to form suspension for later use; dissolving the chloride into the purified water to obtain a chloride solution; filling into a constant-pressure titration hopper; adding dropwise into the reaction vessel accommodating the suspension for later use and reacting; and after the reaction is finished, performing treatment to obtain theproduct amifostine. The amifostine is synthesized by the technical scheme, so yield is high, reaction time is short, cost is low and the preparation method is easy to control and suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of medicine, in particular to a preparation method of amifostine. Background technique [0002] Amifostine belongs to an injection that can be used as an adjuvant therapy for tumor radiotherapy or cytotoxic chemotherapy. The drug is a normal cell protector and is mainly used for adjuvant therapy of various cancers. Applying this drug before chemotherapy for lung cancer, ovarian cancer, breast cancer, nasopharyngeal cancer, bone tumor, digestive tract tumor, blood system tumor and other cancer patients can significantly reduce the damage caused by chemotherapy drugs to the kidney, bone marrow, heart, Ear and nervous system toxicity, and does not reduce the efficacy of chemotherapy drugs. Application of the drug before radiotherapy can significantly reduce the occurrence of xerostomia and mucositis. [0003] Up to now, according to relevant literature reports, there are two main methods for synthesizing am...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/165
Inventor 张宝国王艳侨
Owner KAIFENG MINGREN PHARMA
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