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Cyclovirobuxinum D crystal, its mono-methanol crystal, and preparation and use thereof

A ring-dimensional buxillus, crystal technology, applied in the field of growth of two kinds of crystals

Active Publication Date: 2005-03-16
高华 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In other literatures, the reported ring-dimensional boxwood star D (Xuyangning) crystals are generally needle-like crystals, but none of their three-dimensional dimensions exceeds the millimeter level, and most of the one-dimensional dimensions exceed the millimeter level.

Method used

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  • Cyclovirobuxinum D crystal, its mono-methanol crystal, and preparation and use thereof
  • Cyclovirobuxinum D crystal, its mono-methanol crystal, and preparation and use thereof
  • Cyclovirobuxinum D crystal, its mono-methanol crystal, and preparation and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0082] Embodiment 1 (preparation 1 of Cyclovir buxicine D-methanol crystals)

[0083] Take 1 part of the commercially available raw material of Cyclovitamin D, add 22 parts of pure methanol (w / w or w / v), heat and reflux on a water bath at 80°C for 15 minutes, and suction filter while it is hot. The filtrate at 60°C is heated at 0.5°C / hr cooling rate to 45°C, if necessary, add a small amount of seed crystals, then cool down to 15-25°C at a rate of 4°C / hr, and gradually grow into a rectangular block. If necessary, the temperature can also be reduced to 4 ~8 ℃ cold room temperature carries out crystal growth.Suction filtration, obtains the product of the primary recrystallization of cycloviric buxaxin D-methanol crystal, yield is about about 40%, mother liquor can be used as another solution of primary recrystallization, with The yield of another recrystallization of the solution can reach more than 80%.

[0084] The TLC system 1 and 2 mentioned earlier in this patent are used ...

Embodiment approach 2

[0088] Embodiment 2 (preparation 2 of cyclovir buxicine D-methanol crystals)

[0089] Select pure methanol: the mixed solvent of ethanol=99~85:1~15 as the solvent of recrystallization purification, cooling rate is that room temperature is naturally placed to about 20 ℃ or cooling rate is 0.2~8 ℃ / hr, other conditions are the same as embodiment 1 .

Embodiment approach 3

[0090] Embodiment 3 (preparation 3 of Cyclovir buxicine D-methanol crystals)

[0091]Select a mixed solvent of pure methanol: ethyl acetate = 99-85: 1-15 as the solvent for recrystallization and purification, and the cooling rate is at room temperature and naturally placed to about 20°C or the cooling rate is 0.2-8°C / hr, and other conditions are the same Embodiment 1.

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Abstract

The invention discloses a cyclovirobuxinum D crystal with a molecular formula of C27H50N2O2 belonging to monoclinic crystal system and space group P2(1). The process for preparing crystalline consists of dissolving the market available cyclovirobuxinum D into organic solvent, carrying out solution growth by the mode of recrystallization, wherein the solvent include at least 80 wt% of methanol. The invention also discloses two typeso of cyclovirobuxinum D crystal.

Description

technical field [0001] The present invention relates to ring virbuxin D crystal, its methanol crystal, its preparation method and its use in medicine. The invention further relates to methods of growing both crystals. technical background [0002] Cyclovirobuxinum D (Cyclovirobuxinum D) (also known as boxylarine, epiphylline, etc.) is a drug for treating cardiovascular diseases or as a precursor for new drug development and can be widely used in the medical field. Cyclovitamin D (molecular formula is C 26 h 46 N 2 O) It can be extracted and purified from Buxus microphylla Sieb.etZucc.var.sinica Rehd.et Wils. and plants of the same genus. This product is included in "Chinese Pharmacopoeia" (2000 edition one) as Chinese herbal medicine. [0003] Cycloviral Buxus D is an active ingredient of medicine extracted from the woody part of Buxus microphylla. Chinese boxwood, also known as melon seed boxwood, has the title of millennium dwarf, red day an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K9/00A61K31/57A61P9/00A61P9/10C07J53/00
Inventor 王孟昉李思思何娟杨勇高艺歌
Owner 高华
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