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Method for preparing high-purity high-yield oxysophoridine

A high-yield technology of oxidative sophoridine, applied in the direction of organic chemistry and the like, can solve the problems of low product yield and the like, and achieve the effects of high product purity, simple preparation process and low cost

Inactive Publication Date: 2013-01-09
NINGXIA BAUHINIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of technique for preparing oxidized sophodine from Sophora sophora in order to overcome the defects of existing technology and low product yield, and its purity can reach more than 99% and the yield is also obtained. improvement

Method used

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  • Method for preparing high-purity high-yield oxysophoridine

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Experimental program
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Effect test

Embodiment 1

[0024] Add a certain amount of purified water into the oxidation tank, raise the temperature of the water bath to about 75°C, measure and add 20kg of hydrogen peroxide and stir to make it evenly mixed, then slowly add 40kg of sophoridine and stir to dissolve it, then lower the temperature to 58°C and react at a constant temperature for 7.5 hour, after detecting that there is no hydrogen peroxide in the reaction solution, extract the unreacted sophoridine with toluene until there is no sophoridine in the oxidizing solution, then concentrate under reduced pressure in vacuum, then dissolve with ethanol, and the solution is passed through alumina (Al 2 o 3 ) decolorization, suction filtration, recovery, stirring with acetone, cooling and crystallization, centrifugation to obtain 38 kg of crude product of sophodine oxide, and finally recrystallization to obtain 37.1 kg of refined product of sophodine oxide, with a content of 99.1%.

[0025]

Embodiment 2

[0027] Add a certain amount of purified water into the oxidation tank, raise the temperature of the water bath to about 75°C, measure and add 20kg of hydrogen peroxide and stir to make it evenly mixed, then slowly add 40kg of sophoridine and stir to dissolve it, then lower the temperature to 58°C for constant temperature reaction 8 hour, after detecting that there is no hydrogen peroxide in the reaction solution, extract the unreacted sophoridine with petroleum ether until there is no sophoridine in the oxidizing solution, then concentrate under reduced pressure in vacuum, then dissolve with ethanol, and the solution is passed through alumina (Al 2 o 3 ) decolorization, suction filtration, recovery, stirring with acetone, cooling and crystallization, centrifugation to obtain 38.2 kg of crude product of sophodine oxide, and finally recrystallization to obtain 37.4 kg of fine product of sophodine oxide, with a content of 99.4%.

Embodiment 3

[0029] Add a certain amount of purified water into the oxidation tank, raise the temperature of the water bath to about 75°C, measure and add 20kg of hydrogen peroxide and stir to make it evenly mixed, then slowly add 40kg of sophoridine and stir to dissolve it, then lower the temperature to 60°C for constant temperature reaction 7 hours, after detecting that there is no hydrogen peroxide in the reaction solution, extract the unreacted sophoridine with petroleum ether until there is no sophoridine in the oxidized solution, then concentrate under reduced pressure in vacuo, add ethanol to dissolve, the solution is decolorized by activated carbon, and suction filtered. Recover, add acetone to stir, cool and crystallize, and centrifuge to obtain 38 kg of crude sophodine oxide, and finally recrystallize to obtain 36.8 kg of refined sophodine oxide, with a content of 99.0%.

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Abstract

The invention provides a method for preparing high-purity high-yield oxysophoridine. The preparation method comprises the following steps of: heating purified water in an oxidation tank to a certain temperature in water bath; adding hydrogen peroxide; uniformly mixing by stirring; slowly adding sophoridine; stirring until the sophoridine is dissolved; after hydrogen peroxide is completely reacted at a certain temperature, extracting residual sophoridine by using benzene or ether to obtain a reacted solution; concentrating the reacted solution under reduced pressure to obtain a concentrated solution; adding alcohol to dissolve the concentrated solution; decoloring a solution by adding a decoloring agent; performing suction filtration on the decolored solution to obtain filtrate; concentrating the filtrate under reduced pressure; adding ketone substances and performing crystallization to obtain a coarse product of oxysophoridine; and performing re-crystallization to obtain purified oxysophoridine. The process method is simple and practical and is applied to industrialized production, the cost is low, the purity is high, and the product yield is high.

Description

technical field [0001] The invention relates to a method for preparing oxidized sophoridine with high purity and high yield. Background technique [0002] Oxidized sophoridine (sophoridine) is an alkaloid extracted and isolated from the leguminous plant Sophora sophora, and is the main active ingredient of Chinese herbal medicine. Sophora alopecuroides is the dry aerial part of the leguminous plant Sophora alopecuroides L. The molecular formula is: C 15 h 24 N 2 o 2 , white thick needle crystal or large prism crystal, bitter taste, easily soluble in purified water, methanol, ethanol, carbon tetrachloride, etc. Pharmacological effects: ①Intravenous injection can cause blood pressure to rise first and then drop; ②Excitate the isolated heart of warm-blooded and cold-blooded animals; ③It can cause the contraction of peripheral blood vessels and visceral blood vessels. Through pharmacology and toxicology and clinical research and observation, it is found that the curative...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/22
Inventor 白锋云张勇汪晓东陈殿河
Owner NINGXIA BAUHINIA PHARMA
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