Dammarene diol trimethanol compound, crystal form A and preparation method thereof

A technology of damarene diol and alcoholate, applied in steroids, organic chemistry methods, organic chemistry and other directions, can solve the problems such as the research report on the crystalline form of damarene diol and its preparation method that have not been retrieved, and the like, Achieve the effect of good market prospect, high dissolution and easy dissociation

Active Publication Date: 2020-08-11
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Research reports on the crystal form of dammarenediol and its preparation method have not yet been retrieved

Method used

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  • Dammarene diol trimethanol compound, crystal form A and preparation method thereof
  • Dammarene diol trimethanol compound, crystal form A and preparation method thereof
  • Dammarene diol trimethanol compound, crystal form A and preparation method thereof

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Effect test

Embodiment 1

[0041] Embodiment 1 Preparation of dammarene diol trimethanolate crystal form A

[0042] Add 1 g of dammarene diol into 12 ml of methanol, sonicate for 0.5 h, dissolve, and filter with suction. The sample liquid crystallizes naturally at room temperature for 36 h, filters, and vacuum-dries the filter cake to obtain the needle-shaped dammarene diol trimethanol crystal form. a.

Embodiment 2

[0043] Embodiment 2 Preparation of dammarene diol trimethanolate crystal form A

[0044] Add 1 g of dammarene diol into 5 ml of methanol, sonicate for 0.5 h, dissolve, and filter with suction. The sample liquid crystallizes naturally at room temperature for 12 h, filters, and vacuum-dries the filter cake to obtain the needle-shaped dammarene diol trimethanol crystal form. a.

Embodiment 3

[0045] The preparation of embodiment 3 dammarene diol trimethanol compound

[0046] Add 1 g of dammarene diol into 1 ml of methanol, sonicate for 0.5 h, dissolve, and filter with suction. The sample liquid crystallizes naturally at room temperature for 24 h, filters, and vacuum-dries the filter cake to obtain the needle-shaped dammarene diol trimethanol crystal form. a.

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Abstract

The invention discloses a dammaren diol trimethanol compound, a crystal form A and a preparation method of the dammaren diol trimethanol compound. The X-ray powder diffraction pattern comprises X-raydiffraction peaks as shown at the following 2 theta angles: 6.58 + / -0.2 degrees, 13.35 + / -0.2 degrees, 15.45 + / -0.2 degrees, 20.18 + / -0.2 degrees and 21.83 + / -0.2 degrees. The preparation method disclosed by the invention is safe, simple and convenient, and the prepared dammaren diol trimethanol compound or crystal form A is good in dissolution, high in bioavailability, good in stability, suitablefor drug development and good in marketization prospect.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, in particular relates to a dammarene diol trimethanol compound and its crystal form, and specifically discloses a preparation method thereof. Background technique [0002] Dammarenediol (Dammarenediol II) is a precursor for the synthesis of protopanaxadiol, which can be derived from protopanaxadiol. Cytochrome P450 participates in the hydroxylation of dammarenediol C12 to form protopanaxadiol, and the C6 site of protopanaxadiol is hydroxylated by cytochrome P450 to obtain protopanaxatriol. These two compounds are the main molecular framework of ginsenosides. [0003] [0004] Chinese patent CN201310129592.2 discloses a method for the biosynthesis of dammarene diol, in which a recombinant strain is constructed by means of genetic engineering to produce dammarene diol. [0005] Chinese patent CN201810781608.0 obtains the recombinant Saccharomyces cerevisiae which uses xylose to pro...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07B2200/13C07J9/00
Inventor 梁红宝朱峰
Owner LUNAN PHARMA GROUP CORPORATION
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