Unlock instant, AI-driven research and patent intelligence for your innovation.

Nelarabine crystalline compound and preparation method thereof

A compound and crystallization technology, applied in the field of nerabine crystalline compounds and their preparation, can solve the problems of limited application, poor solubility of nerabine and the like

Active Publication Date: 2015-07-08
山东罗欣乐康制药有限公司 +3
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the poor solubility of nelarabine in water, this limits its application in medicine to a certain extent.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Nelarabine crystalline compound and preparation method thereof
  • Nelarabine crystalline compound and preparation method thereof
  • Nelarabine crystalline compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Get 25.0 g of commercially available nalarabine crude drug and put it into 800 ml of anhydrous methanol, heat to reflux for 2 hours, the crude product of nalarabine is basically dissolved, then add 1 gram of activated carbon and reflux for 15 minutes, filter while it is hot, drop to room temperature, and store on ice Cool the salt bath to -5°C, crystallize, filter with suction, and wash the filter cake with a small amount of ice methanol to obtain 11.6 g of fine nelarabine, which is the crystalline compound of nelarabine.

[0068] The obtained nelarabine crystalline compound is subjected to the following X-ray powder diffraction analysis:

[0069] Sample treatment: the prepared nelarabine crystalline compound was ground and passed through a 100-mesh sieve, and 50 mg was weighed as a sample for powder X-ray diffraction experiment.

[0070] Experimental instrument: Japan Rigaku D / max-2550 powder X-ray diffractometer.

[0071] Experimental conditions: CuK α Radiation, gr...

Embodiment 2

[0078] Get 25.0g of commercially available nalarabine crude drug and drop it in 750ml of anhydrous methanol, heat to reflux, stir for 3 hours, and the nalarabine basically dissolves, then add 1 gram of activated carbon and reflux for 10 minutes, filter while it is hot, and drop to room temperature, Cool down to 0°C in an ice-salt bath, crystallize, filter with suction, and wash the filter cake with a small amount of ice methanol to obtain 11.8 g of fine nelarabine, which is the crystalline compound of nelarabine.

Embodiment 3

[0080] Take 25.0 g of nalarabine crude product and put it into 875 ml of anhydrous methanol, heat to reflux, stir for 1 hour, and the nalarabine is basically dissolved, then add 1 g of activated carbon and reflux for 20 minutes, filter while it is hot, drop to room temperature, and cool down in an ice-salt bath At -3°C, crystallize, filter with suction, and wash the filter cake with a small amount of ice methanol to obtain 11.9 g of fine nelarabine, which is the crystalline compound of nelarabine.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to nelarabine crystalline compound and a preparation method thereof. The crystalline compound is measured by a powder X-ray diffraction method; and the obtained X-ray powder diffraction pattern is shown in a figure; the nelarabine crystalline compound is a novel crystal form which is different from that in the prior art; and the crystal form has obviously improved dissolubility in water. The invention also relates to a preparation method of the crystalline compound. The preparation method comprises the following steps of: taking and putting a nelarabine crude product into absolute methanol, heating and refluxing; adding active carbon for refluxing after dissolving the nelarabine crude product; filtering at high temperature, cooling to room temperature, cooling by virtue of ice salt bath, devitrifying and performing suction filtration, and washing a filter cake by ice methanol to obtain the nelarabine crystalline compound. The method disclosed by the invention is simple and convenient to operate, and is a method which is economical, and feasible, and suitable for industrial purification.

Description

technical field [0001] The invention relates to the crystallization of nucleoside compounds and a preparation method thereof, in particular to a nelarabine crystalline compound and a preparation method thereof. Background technique [0002] Nelarabine is the prodrug of the deoxyguanosine analogue 9-β-D-arabinofuranosylguanine (ara-G), which was approved for marketing in 2005 and can be used for the treatment of T-cell acute lymphoblastic leukemia (T -ALL) and T-cell lymphoblastic lymphoma (T-LBL). [0003] Nelarabine has the following structural formula, and its chemical name is 2-amino-9-β-D-arabinofuranosyl-6-methoxy-9H-purine. [0004] [0005] Nelarabine is white or off-white crystalline powder, slightly soluble in water, the solubility in water is about 8-9mg / ml (25℃, pH=4-10). Due to the poor solubility of nelarabine in water, this limits its application in medicine to a certain extent. [0006] CN101348511A discloses the synthesis and refining of nelarabine, whe...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/19C07H1/06
Inventor 朱玉青李明杰韩风生李志滨王兴玉
Owner 山东罗欣乐康制药有限公司