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Synthesis technology ofminoxidil

A synthesis process and reaction kettle technology, applied in the field of pharmaceutical synthesis, can solve problems such as low yield and complexity, and achieve the effects of mature production process, low pollution and high yield

Active Publication Date: 2017-10-10
安徽拜善晟制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In China, there are few reports on the synthesis of minoxidil, and the synthesis process of minoxidil abroad is relatively complicated and the yield is not high

Method used

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  • Synthesis technology ofminoxidil
  • Synthesis technology ofminoxidil
  • Synthesis technology ofminoxidil

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Experimental program
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Effect test

Embodiment Construction

[0048] A kind of synthetic technique of minoxidil, comprises the following steps:

[0049] The first step: oxidation reaction generates intermediate 2,6-diamino-4-chloropyrimidine-1-oxide,

[0050] One: Reaction Equation

[0051]

[0052] Two: material ratio table

[0053]

[0054]

[0055] Three: specific operation

[0056] 1. Add 310kg of chloroform into a clean 2T reaction kettle, and the temperature inside the kettle is 17°C;

[0057] 2. Slowly add 150.0 kg of 2,4-diamino-6-chloropyrimidine solid, there is a slight exotherm when adding, and there is no need to use an ice-water bath to cool down;

[0058] 3. Heating to reflux;

[0059] 4. Add 620kg of chloroform and 189kg of m-chloroperoxybenzoic acid into another clean 2T reaction kettle to release heat without using an ice-water bath to cool down;

[0060] 5. Pump the chloroform solution of m-chloroperoxybenzoic acid into the high-level tank, and add it dropwise to the chloroform solution of 2,4-diamino-6-ch...

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Abstract

The invention discloses a synthesis technology of minoxidil. The technology comprises steps as follows: firstly, meta-chloroperoxybenzoic acid is utilized to oxidize 2,4-diamino-6-chloropyrimidine, 2,6-diamino-4-chloropyrimidine-1-oxide as an intermediate is obtained, then 2,6-diamino-4-chloropyrimidine-1-oxide as the intermediate is subjected to condensation with piperidine under the alkaline condition, and a crude product of minoxidil is obtained; finally, the crude product of minoxidil is crystallized in isopropanol and purified, and a refined finished minoxidil product is obtained. The technology adopts a simple principle and is convenient to operate, and the product is high in yield and good in purity.

Description

technical field [0001] The invention relates to the field of medicine synthesis, in particular to a synthesis process of minoxidil. Background technique [0002] Minoxidil, also known as Changyading, Minoxidine, molecular formula and relative molecular mass C9H15N5O=209.25, is white or off-white crystalline powder, slightly soluble in water or chloroform, slightly soluble in ethanol, slightly soluble in acetone, soluble in glacial acetic acid. It can directly act on the blood vessel wall, dilate small arteries, reduce peripheral resistance, lower blood pressure, and increase heart rate and cardiac output, but its antihypertensive effect is more significant and lasting than that of hydralazine. [0003] Dilute solutions of minoxidil, as an effective drug for the treatment of hair loss, have received widespread attention. In today's society, due to the accelerated pace of life, people's pressure is increasing, resulting in more and more hair loss patients, and the demand for...

Claims

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Application Information

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IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 常松王喆明何万通慕龙治范征吴章栓
Owner 安徽拜善晟制药有限公司
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