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Preparation method high-purity high-yield oxysophocarpine

A technology of oxidative sophocarpine and high yield, applied in the direction of organic chemistry and the like, to achieve the effects of high yield, simple preparation process and high quality

Inactive Publication Date: 2013-01-02
NINGXIA BAUHINIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Oxidized sophocarpine has very high medicinal value, and its industrial preparation method is rarely reported in the patent literature. Although the preparation method of oxidized sophocarpine disclosed by CN1354181A and CN1935809 has its advanced technology, in specific operations, such as There is still a lot of room for improvement in the refinement of its process

Method used

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  • Preparation method high-purity high-yield oxysophocarpine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add water to the oxidation tank and raise the temperature of the water bath to about 75°C, measure and add 20kg of hydrogen peroxide, slowly add 40kg of sophocarpine, and dissolve;

[0024] (2) Reduce the temperature to 62°C for 7.5 hours at a constant temperature, and detect that there is no hydrogen peroxide;

[0025] (3) Extract unreacted sophocarpine with toluene until there is basically no sophocarpine in the oxidation solution;

[0026] (4) Concentrate the reaction solution under reduced pressure in vacuo, add ethanol to dissolve, and filter with suction;

[0027] (5) The filtrate is passed through alumina (Al 2 o 3 ) for decolorization, suction filtration, and recovery;

[0028] (6) Stir with acetone, cool and crystallize, and centrifuge to obtain 38.8 kg of crude sophocarpine oxide;

[0029] (7) 37.6kg of fine oxidized sophocarpine was obtained by recrystallization of the crude product of oxidized sophocarpine, and the content was determined to be 99.6%....

Embodiment 2

[0031] (1) Add water to the oxidation tank and raise the temperature of the water bath to about 75°C, measure and add 20kg of hydrogen peroxide, slowly add 40kg of sophocarpine, and dissolve;

[0032] (2) Reduce the temperature to 60°C for 8 hours, and detect the absence of hydrogen peroxide;

[0033] (3) Extract unreacted sophocarpine with ether until there is basically no sophocarpine in the oxidation solution;

[0034] (4) Concentrate the reaction solution under reduced pressure in vacuo, add ethanol to dissolve, and filter with suction;

[0035] (5) The filtrate is decolorized by activated carbon, filtered and recovered;

[0036] (6) Add acetone to stir, cool and crystallize, and centrifuge to obtain 38 kg of crude product of oxysophocarpine;

[0037] (7) 37.1kg of fine oxidized sophocarpine was obtained by recrystallization of the crude product of oxidized sophocarpine, and the content was determined to be 99.1%.

Embodiment 3

[0039] (1) Add water to the oxidation tank and raise the temperature of the water bath to about 75°C, measure and add 20kg of hydrogen peroxide, slowly add 40kg of sophocarpine, and dissolve;

[0040] (2) Reduce the temperature to 58°C for 8.5 hours at a constant temperature, and detect that there is no hydrogen peroxide;

[0041] (3) Extract unreacted sophocarpine with benzene until there is basically no sophocarpine in the oxidation solution;

[0042] (4) Concentrate the reaction solution under reduced pressure in vacuo, add ethanol to dissolve, and filter with suction;

[0043] (5) The filtrate is passed through alumina (Al 2 o 3 ) for decolorization, suction filtration, and recovery;

[0044] (6) Stir with acetone, cool and crystallize, and centrifuge to obtain 38.5 kg of crude product of oxysophocarpine;

[0045] (7) 37.5kg of fine oxidized sophocarpine was obtained by recrystallization of the crude product of oxidized sophocarpine, and the content was determined to b...

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Abstract

The invention provides a preparation method high-purity high-yield oxysophocarpine. The method comprises the following steps: firstly heating purified water in a water bath to a certain temperature, adding hydrogen peroxide, slowly adding sophocarpine, reacting at a certain temperature till hydrogen peroxide is completely consumed, then extracting the residual small amount of sophocarpine; performing reduced pressure concentration of the reaction solution, adding alcohol substances into the concentrate for dissolution, adding alumina for decoloring, performing suction filtration; continuing to perform reduced pressure concentration, adding ketone substances for crystallization, and performing recrystallization to obtain oxysophocarpine. The process method is simple and practical, low in cost, high in purity, high in yield, and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing oxidized sophocarpine with high purity and high yield. Background technique [0002] Oxysophocarpine is an alkaloid isolated from Sophra flavescens Ait (Sophra flavescens Ait) or Sophora subprostrata chrnet T. Chen, and is the main active ingredient of Chinese herbal medicine. Molecular formula: C 15 h 22 N 2 o 2 , is white or off-white crystalline powder, odorless and bitter. It can increase the number of white blood cells, strengthen the body's immunity, and play the role of resisting Shigella, dermatophytes, amoeba, trichomonas and other infections. Oral administration can treat acute bacillary dysentery, tonsillitis, mastitis, pelvic inflammatory disease, lymphadenitis, bronchitis, wheezing, arrhythmia, low leukocytes, etc. It is also effective for psoriasis and insomnia. [0003] Oxidized sophocarpine has very high medicinal value, and its industrial preparation method is rarely reported in the...

Claims

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Application Information

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