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Entecavir kalium, preparation method and application thereof

A technology of Entecavir and Cavir Potassium, which is applied in the field of potassium salt compound of Entecavir and its preparation, can solve the problems of improvement, low solubility of Entecavir in water, unfavorable preparation of oral preparations and bioavailability, and achieve good therapeutic effect and good water solubility performance effect

Inactive Publication Date: 2008-06-11
CHANGZHOU NO 4 PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Because the water solubility of entecavir is very small, it is not conducive to the preparation of oral preparations and the improvement of bioavailability

Method used

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  • Entecavir kalium, preparation method and application thereof
  • Entecavir kalium, preparation method and application thereof
  • Entecavir kalium, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1. Preparation of Entecavir Potassium

[0028] Take 5 grams of Entecavir, add potassium hydroxide aqueous solution to dissolve, adjust the pH value to 11, add about 65ml of ethanol while stirring, continue stirring for 10 minutes, let stand for 2 hours, filter with suction, and wash the filtered precipitate with ethanol for 2 to 3 times Afterwards, adopt vacuum drying method, dry at 60 ℃ for 4 hours, obtain off-white solid powder, be entecavir potassium, molecular formula C 12 h 14 N 5 o 3 K, elemental analysis result (%): C 45.76, H 4.44, N 22.27, K 12.36, theoretical value (%): C 45.70, H 4.47, N 22.21, K 12.40, elemental analysis value is consistent with theoretical value.

[0029] NMR analysis 1 H-NMR δ(ppm) (400MHZ, DMSO): 1.79-2.04 (2H, multiplet), 2.0 (1H, singlet), 2.33 (1H, multiplet), 3.24 (1H, multiplet), 3.40-3.65 (2H, multiplet), 4.37 (1H, multiplet), 4.87 (1H, doublet), 4.95 (1H, doublet), 8.68 (1H, doublet).

Embodiment 2

[0030] Example 2. Preparation of Entecavir Potassium Crystal Hydrate

[0031] Take 5 grams of Entecavir, add potassium hydroxide aqueous solution to dissolve, adjust the pH value to 13, add about 70ml of acetone and ethanol mixed solution (V:V=1:1) under stirring, continue stirring for 10 minutes, let stand for 2 hours, pump After filtering, the filtered precipitate was washed with ethanol for 2 to 3 times, dissolved in water, and vacuum dried at 60°C for 4 hours to obtain an off-white solid.

[0032] According to thermogravimetric and differential thermal analysis, it contains a molecule of crystal water, which is entecavir potassium monohydrate, molecular formula C 12 h 14 N 5 o 3 K·H 2 O.

[0033] Elemental analysis results (%): C 43.20, H 4.88, N 21.06, K 11.68, theoretical values ​​(%): C 43.23, H 4.84, N 21.01, K 11.73, elemental analysis values ​​are consistent with theoretical values.

[0034] NMR analysis H 1 -NMR δ (ppm) (400MHZ, DMSO): 1.78-2.05 (2H, multiple...

Embodiment 3

[0035] Embodiment three. the preparation of entecavir potassium tablet

[0036] Get 1.15 grams of Entecavir Potassium prepared in Example 1, add an appropriate amount of carrier auxiliary materials (such as starch, lactose, mannitol, dextrin, hydroxypropyl cellulose, povidone, magnesium stearate, etc.), wet granulation, drying Dry, compress into tablets with a tablet machine, each tablet has a specification of 0.5mg (calculated as entecavir), for oral use.

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Abstract

The invention relates to medicine technical field, in particular to a sylvite compound of entecavir, a relative preparation method and medical application thereof. The invention dissolves entecavir in a tic potash water solution to be reacted, deposits via unit alcohol or ketone with low carbon chains, dries and purifies to obtain the product. The entecavir sylvite has high solubility, for supporting drug preparation and improving drug bioavailability. The entecavir sylvite can improve the sylvite supplementary of hepatopath and adjust electrolyte balance disorder of hepatitis patient, with high clinical value.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular to a potassium salt compound of entecavir, a preparation method thereof and an application thereof in medicine. Background technique [0002] Entecavir (Entecavir) is a 2'-pentanecyclodeoxyguanosine analogue, Entecavir is a chiral compound, in which the [1s-(1α, 3α, 4β) conformation has extremely strong anti-hepatitis B virus capacity, and its raw materials and preparations are currently on the market. The molecular structural formula of Entecavir is as follows: [0003] [0004] Molecular formula C 12 h 15 N 5 o 3 . [0005] Because the water solubility of entecavir is very small, it is not conducive to the preparation of oral preparations and the improvement of bioavailability. Contents of the invention [0006] The technical problem to be solved by the present invention is to overcome the above disadvantages, research and design entecavir derivatives with good water ...

Claims

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Application Information

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IPC IPC(8): C07D473/18A61K31/513A61P1/16A61P31/12
Inventor 庄苏静屠永锐
Owner CHANGZHOU NO 4 PHARMA FACTORY
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