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Pumiloside preparation method

A kind of technology of scutellarin and isovinblastin lactam, applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry and other directions, can solve the difficulty of separating and purifying scutellarin, problems such as low content, to achieve the effect of simple operation and wide source of raw materials

Active Publication Date: 2016-01-27
JIANGSU KANION PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the main source of brachyrrhizin is the separation and extraction of brachyrrhizin, but the content of brachyrrhizin in gallwood is relatively low, and it is difficult to separate and purify brachyrrhizin from gallwood

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Study on the light irradiation stability of vinca lactam aqueous solution

[0045] Take an appropriate amount of vinca lactam, dissolve it with ultrapure water ultrasonically to prepare a solution of about 1.2mg / ml, filter, and divide the filtrate into 10ml vials, divide them into three groups, the first group is added to the solution Filled with nitrogen, the second group was filled with oxygen into the solution, the third group was air, plugged, capped, and sterilized (temperature: 121°C; time 20min). Due to the long light time, in order to eliminate the influence of microorganisms, it is preferable to perform high temperature sterilization on the vinca lactam solution. Samples were taken after the samples were placed at room temperature. The vinca lactam content in the samples before and after sterilization was detected by HPLC, and then the three groups of samples were stored at room temperature under natural light and dark place. After 7 days, samples were ...

Embodiment 2

[0051] Weigh 0.7g of vinca lactam raw material, dissolve it with 500ml ultrapure water ultrasonically, filter, and divide the filtrate into 20ml vials, fill with oxygen, stopper, cap, and sterilize (temperature: 121℃; Time 20min). The sample is placed in natural light for 7 days, the reaction solution is passed through the HPD100 macroporous adsorption resin column, and eluted with water, 20% ethanol, 40% ethanol successively, and the 40% ethanol eluate is collected, concentrated and dried to obtain the main degradation Things ( figure 1 No. 1 and No. 2 chromatographic peaks) dry paste 262mg; the dry paste is dissolved in methanol and separated by liquid phase preparation, the mobile phase is acetonitrile-water (15:85), and the chromatographic peaks No. 1 and No. 2 are collected respectively The eluent. The separated degradation product No. 1 is unstable in the eluent, and it is still difficult to obtain an eluent containing a single chromatographic peak (see figure 2 ). In...

Embodiment 3

[0054] Weigh 0.7g of vinca lactam raw material, dissolve it with 500ml ultrapure water ultrasonically, filter, and divide the filtrate into 20ml vials, continue to infuse oxygen, sterilize at 100℃ for 60min, then place the sample in natural light After standing for 7 days, the reaction solution was passed through the HPD100 macroporous adsorption resin column, and then eluted with water, 20% ethanol, 40% ethanol in sequence, collected the 40% ethanol eluate, concentrated and dried to obtain 0.6 g of crude product, which was crystallized with methanol , To obtain white rod-shaped crystals with a yield of 70% and a purity of 90%. The structure of the obtained crude product was identified, and the result was the same as in Example 2.

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Abstract

The present invention belongs to the field of pharmaceutical chemistry, and discloses a pumiloside preparation method. According to the pumiloside preparation method, strictosamide is adopted as a raw material, and is subjected to illumination placing under an oxygen-containing sealing condition to obtain pumiloside. According to the present invention, the strictosamide content in nauclea officinalis is high, and a column chromatography method is used to separate so as to obtain the strictosamide, such that the raw material sources of the method are wide; and the preparation method has characteristics of simple operation and green environmental protection, and the pumiloside yield is more than 70%.

Description

Technical field [0001] The present invention belongs to the field of medicinal chemistry, and specifically relates to a method for preparing brevis root, in particular to a method for preparing brevis root by using isovinca lactam as a raw material. Background technique [0002] Naucleaofficinalis Pierreex Pitard is a tree of the genus Ebony in the Rubiaceae family. It is also known as ebony, mountain bear bile, and bear bile tree. It is mainly distributed in Guangdong, Guangxi, Hainan and other regions. It is one of the rare wild plant species under protection in my country. Gallbladder is used as medicine with branches, stems, and skins. It has a bitter taste and cold nature. Commonly used in southern my country for the treatment of cold and fever, acute tonsillitis, pharyngitis, mastitis, pneumonia, enteritis, dysentery, eczema, rash, abscess, urinary tract infection, cholecystitis, lower limb ulcer, athlete's foot infection and other diseases, but also Blindly taste the commo...

Claims

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Application Information

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IPC IPC(8): C07H17/00C07H1/00
Inventor 萧伟王振中丁岗李兆亮刘文君孟兆青孙林杨彪齐晓辉
Owner JIANGSU KANION PHARMA CO LTD
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