Dammarenediol ethyl acetate compound, crystal form i and preparation method thereof

A technology of dammarene diol ethyl acetate and dammarene diol, which is applied in the direction of carboxylic acid ester preparation, organic compound preparation, steroidal compounds, etc., and can solve the problem of dammarene diol crystal form and research reports on its preparation methods, etc., to achieve good market prospects, broaden clinical applications, and good stability

Active Publication Date: 2021-06-22
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there are no research reports on the crystal form of dammarenediol and its preparation method

Method used

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  • Dammarenediol ethyl acetate compound, crystal form i and preparation method thereof
  • Dammarenediol ethyl acetate compound, crystal form i and preparation method thereof
  • Dammarenediol ethyl acetate compound, crystal form i and preparation method thereof

Examples

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Effect test

Embodiment 1

[0040] Embodiment 1 Preparation of dammarene diol ethyl acetate compound crystal form I

[0041] Add 1 g of dammarene diol into 8 ml of ethyl acetate, heat and reflux to dissolve for 15 hours, and filter with suction. The sample liquid crystallizes naturally at room temperature for 12 hours, filters, and vacuum-dries the filter cake to obtain flaky dammarene diol ethyl acetate Form I.

Embodiment 2

[0042] The preparation of embodiment 2 dammarene glycol ethyl acetate compound

[0043] Add 1g of dammarene diol into 4ml of ethyl acetate, heat and reflux to dissolve for 3h, suction filter, the sample liquid crystallizes naturally at room temperature for 5h, filter, and vacuum dry the filter cake to obtain flaky dammarene diol ethyl acetate Form I.

Embodiment 3

[0044] The preparation of embodiment 3 dammarene glycol ethyl acetate compound

[0045] Add 1 g of dammarene diol into 1 ml of ethyl acetate, heat and reflux to dissolve for 3 hours, filter with suction, and crystallize the sample liquid at room temperature for 8 hours, filter, and dry the filter cake in vacuum to obtain flaky dammarene diol ethyl acetate Form I.

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Abstract

The invention discloses a dammarenediol ethyl acetate compound, crystal form I and a preparation method thereof. The present invention provides a crystal form A of dammarene diol ethyl acetate compound, whose X-ray powder diffraction pattern includes the following X-ray diffraction peaks shown at 2θ angles: 5.66°±0.2°, 16.97°±0.2 °, 17.52°±0.2° and 44.18°±0.2°. The preparation method of the invention is safe and convenient, and the prepared dammarene diol ethyl acetate compound or crystal form A has good stability, is suitable for drug development, and has good market prospects.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, in particular relates to a dammarene diol ethyl acetate 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 p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00C07C69/14C07C67/52
CPCC07B2200/13C07C67/52C07C69/14C07J9/00
Inventor 朱峰宁停波
Owner LUNAN PHARMA GROUP CORPORATION
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