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Preparation of demethylated manganese cantharidate

A technology of manganese methylcantharidinate and methylcantharidin acid, which is applied in the field of preparation of manganese demethylcantharidinate and manganese demethylcantharidinate, can solve the problems of reduced anticancer activity, etc. Achieve the effect of small molecular weight, high purity and good safety

Inactive Publication Date: 2014-07-09
ZUNYI MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when demethylated cantharidin is reduced, its anticancer activity is greatly reduced. This urgently requires the development of other new cantharidin derivatives with higher anticancer activity to solve this problem.

Method used

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  • Preparation of demethylated manganese cantharidate

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Effect test

Embodiment 1

[0013] A preparation method for manganese demethylcantharidinate, comprising the steps of:

[0014] (1) Add 100 ml deionized water to a 100 ml beaker and heat to 70 °C, add

[0015] 0.168 g demethylcantharidin was dissolved by magnetic stirring.

[0016] (2) Add 0.178 g of manganese hydroxide to make the molar ratio of norcantharidin to manganese hydroxide 1:2. Heated and stirred with magnetic force for 30 minutes.

[0017] (3) Centrifuge at 10 000 g for 30 min, discard the precipitate and keep the supernatant. After the supernatant was dried under reduced pressure at 60°C, colorless and irregular crystals were obtained, which was pure manganese demethylcantharidinate.

Embodiment 2

[0019] A preparation method for manganese demethylcantharidinate, comprising the steps of:

[0020] (2) Add 1000 ml deionized water to a 1000 ml beaker and heat to 70 °C, add

[0021] 1.68 g demethylcantharidin was dissolved by magnetic stirring.

[0022] (2) Add 3.56 g of manganese hydroxide to make the molar ratio of norcantharidin to manganese hydroxide 1:4. Heated and stirred with magnetic force for 60 minutes.

[0023] (3) Centrifuge at 10 000 g for 30 min, discard the precipitate and keep the supernatant. After the supernatant was dried under reduced pressure at 60°C, colorless and irregular crystals were obtained, which was pure manganese demethylcantharidinate.

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Abstract

The invention discloses a demethylated manganese cantharidate of which the structural formula (I) is disclosed in the specification. The preparation method comprises the following steps: heating a certain volume of deionized water to 70-80 DEG C, and adding a certain amount of demethylated cantharidin until the end concentration is 12.5 mmol / L; adding a certain amount of manganous hydroxide until the mole ratio of the demethylated cantharidin to the manganous hydroxide is 1:2-1:5; heating while magnetically stirring to react for 30-60 minutes, centrifuging at 10000g for 30 minutes, and discarding the precipitate to reserve the supernatant; and drying the supernatant at 60 DEG C under reduced pressure to obtain the colorless random crystal. The demethylated manganese cantharidate has the characteristics of higher anticancer activity, simple technique, favorable safety, stable finished product performance and high purity, and the preparation method is easy to operate.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to the preparation of manganese demethylcantharidinate and a preparation method of manganese demethylcantharidinate. Background technique [0002] In the first and second centuries, my country began to use mylabris to treat tumors. Later, it was confirmed that the cantharidin and cantharidin derivatives secreted by the cantharidin were the main effective substances. Because cantharidin has good anti-tumor activity, but its toxicity is extremely high, people have changed it through chemical methods, and have successfully synthesized demethylated cantharidin to reduce its toxicity. At present, the demethylated cantharidin has been successfully applied clinically and achieved remarkable results. However, the anticancer activity of demethylated cantharidin is greatly reduced when the concentration is reduced, which urgently requires the development of other new cantharid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08A61K31/34A61P35/00
CPCC07D493/08
Inventor 刘云李晓飞赵长阔晏容刘流侯晓晖
Owner ZUNYI MEDICAL UNIVERSITY
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