Novel valganciclovir crystal form

A technology of crystal form and acetone, which is applied in the field of preparation of raw materials, can solve the problems that valganciclovir is easy to absorb moisture, achieve good anti-hygroscopic performance, avoid crystal form changes and increase the effect of related substances

Inactive Publication Date: 2018-05-25
WEIHAI GUANBIAO INFORMATION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a new crystal form of valganciclovir resistant to moisture absorption, which solves the problem that existing valganciclovir is easy to absorb moisture

Method used

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  • Novel valganciclovir crystal form
  • Novel valganciclovir crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The first step 18g valganciclovir crude product is dissolved in 100ml ethanol-acetone mixed solvent, and in described mixed solvent, the volume ratio of ethanol and acetone is 1:0.3.

[0025] Step 2: At room temperature, add 1.45 g of activated carbon to the solution in Step 1, stir for 1 hour, and filter;

[0026] In the third step, under stirring, the temperature of the filtrate in the second step was lowered to -12°C and kept, and 17ml of acetone was slowly added dropwise at a rate of 0.90ml / min. A white solid was precipitated, and the stirring was continued for 3-5 hours. Stirring speed is 170 rpm;

[0027] The fourth step is to filter, and the filter cake is washed 3 times with absolute ethanol, each dosage is 8ml, the filter cake is spread out, and vacuum-dried at 40°C.

[0028] Obtain crystal formation described in the present invention, its X-ray powder diffraction figure sees attached figure 1 , with a melting point of 280.63°C, a purity of 99.97% detected by...

Embodiment 2

[0030] The first step 26g valganciclovir crude product is dissolved in ethanol-acetone mixed solvent, and in described mixed solvent, the volume ratio of ethanol and acetone is 1:0.6.

[0031] Step 2: At room temperature, add 2.6 g of activated carbon to the solution in Step 1, stir for 1 hour, and filter;

[0032] In the third step, under stirring, the temperature of the filtrate in the second step is lowered to -5°C and maintained, and 25ml of acetone is slowly added dropwise at a rate of 1.5ml / min. A white solid is precipitated, and the stirring is continued for 3-5 hours , the stirring speed is 190 rpm;

[0033] The fourth step is to filter, and the filter cake is washed 3 times with absolute ethanol, each dosage is 10ml, the filter cake is spread out, and vacuum-dried at 40°C.

[0034] Obtain crystal formation described in the present invention, its X-ray powder diffraction figure sees attached figure 1 , with a melting point of 281.01°C, a purity of 99.99% detected by ...

Embodiment 3

[0036] The first step 22g valganciclovir crude product is dissolved in ethanol-acetone mixed solvent, in described mixed solvent, the volume ratio of ethanol and acetone is 1:0.45;

[0037] Step 2: At room temperature, add 2 g of activated carbon to the solution in Step 1, stir for 1 hour, and filter;

[0038] In the third step, under stirring, the temperature of the filtrate in the second step was lowered to -7°C and kept, and 21ml of acetone was slowly added dropwise at a rate of 1.2ml / min. A white solid was precipitated, and the stirring was continued for 3-5 hours. Stirring speed is 180 rpm;

[0039] The fourth step is to filter, and the filter cake is washed 3 times with absolute ethanol, each dosage is 9ml, the filter cake is spread out, and vacuum-dried at 40°C.

[0040] Obtain crystal formation described in the present invention, its X-ray powder diffraction figure sees attached figure 1 , melting point 280.92°C, HPLC purity of 99.99%, yield of 92.14%, particle size ...

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Abstract

The invention relates to a novel valganciclovir crystal form, and belongs to the technical field of preparation of medicinal raw materials. The invention adopts the technical scheme as follows: X-raypowder diffraction of the novel valganciclovir crystal form shows that absorption peaks at positions with 2theta of 8.51, 11.08, 12.30, 13.18, 14.39, 16.81, 17.06, 17.76, 19.28, 19.82, 21.74, 22.81 and 23.56 are relatively strong. The invention provides the novel valganciclovir crystal form with a very good antihygroscopic property, and a stable medicinal raw material is provided for preparing a valganciclovir preparation.

Description

technical field [0001] The invention relates to a new crystal form of valganciclovir, which belongs to the technical field of preparation of raw materials. Background technique [0002] Valganciclovir (Valganciclovir), the chemical name is L-valine, 2-[(2-amino-1,6-dihydro-6-oxo-9H-purin-9-yl)methoxy] -3-Hydroxypropyl ester hydrochloride. Valganciclovir hydrochloride is approved for the treatment of cytomegalovirus (CMV) retinitis in patients with acquired immunodeficiency syndrome (AIDS) and for the prophylaxis of kidney, heart, and kidney-pancreas transplants Potent antiviral agent for CMV disease. Valganciclovir hydrochloride is the L-monovaline ester of ganciclovir and is a stable prodrug of ganciclovir with improved absorption. [0003] Valganciclovir hydrochloride is a white to off-white crystalline powder, the solubility of valganciclovir hydrochloride in aqueous solution is pH dependent, and the maximum solubility in the range of 4-6pH is greater than 200mg / mL. D...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/18
CPCC07D473/18C07B2200/13
Inventor 孙爱梅
Owner WEIHAI GUANBIAO INFORMATION TECH
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