Preparation method of tenofovir alafenamide semifumarate

A technology of tenofovir alafenamide and hemifumarate, which is applied in the field of single crystal preparation, can solve the problems of no single crystal in the cultivation of the compound, difficulty in cultivating single crystal, difficulty in single crystal cultivation, etc., and achieves the goal of preparing The conditions are easy to control, the solution is not easy to cultivate, and the effect of simple operation

Inactive Publication Date: 2018-09-18
CHENGDU BRILLIANT PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, some compounds can easily obtain a certain crystal form, but it is very difficult to grow single crystals, and many compounds cannot even grow single crystals.
The single crystal cultivation of tenofovir alafenamide hemifumarate is very difficult, and th

Method used

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  • Preparation method of tenofovir alafenamide semifumarate
  • Preparation method of tenofovir alafenamide semifumarate
  • Preparation method of tenofovir alafenamide semifumarate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve tenofovir alafenamide and fumaric acid in 30 times the total mass of tenofovir alafenamide and fumaric acid in acetonitrile at room temperature at a molar ratio of 2:1, and the resulting mixture is placed in In the vial, the mouth of the bottle is partially closed so that the solvent can be volatilized, and then placed in an oven at 40°C, volatilized until a transparent cubic single crystal is obtained, and the colorless and transparent tenofovir alafenamide hemifumarate is obtained. Cubic single crystal.

Embodiment 2

[0032] Dissolve tenofovir alafenamide and fumaric acid in 30 times the total mass of tenofovir alafenamide and fumaric acid in acetonitrile at room temperature at a molar ratio of 2:1, and the resulting mixture is placed in In the vial, the mouth of the bottle is partially closed to make the solvent volatilize, and then placed in an oven at 45°C, volatilized until a transparent cubic single crystal is obtained, and a colorless transparent cube of tenofovir alafenamide hemifumarate is obtained single crystal.

Embodiment 3

[0034] Dissolve tenofovir alafenamide and fumaric acid in 30 times the total mass of tenofovir alafenamide and fumaric acid in acetonitrile at room temperature at a molar ratio of 2:1, and the resulting mixture is placed in In the vial, the mouth of the bottle is partially closed to make the solvent volatilize, and then placed in an oven at 55°C, volatilized until a transparent cubic single crystal is obtained, and a colorless transparent cube of tenofovir alafenamide hemifumarate is obtained single crystal.

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Abstract

The invention provides a preparation method of tenofovir alafenamide semifumarate monocrystal. The preparation method comprises the following steps of dissolving tenofovir alafenamide and fumaric acidinto a solvent of the tenofovir alafenamide and the fumaric acid with the total mass time being 20-50 times at room temperature according to a molar ratio being 2 to 1, containing an obtained mixed liquid in a vessel, enabling the solvent to be volatilizable with the vessel not being sealed or partly sealed, then putting the vessel in the environment with a single crystal cultivation temperaturebeing 40-60 DEG C, and enabling the solvent to volatilize until a cuboid or rectangular colorless and transparent monocrystal is obtained. By adopting the preparation method, a tenofovir alafenamide semifumarate monocrystal can be relatively easily prepared, and structure confirmation of the tenofovir alafenamide semifumarate is facilitated.

Description

technical field [0001] The invention belongs to the field of pharmaceutical crystal forms, in particular to the preparation of a single crystal (tenofovir alafenamide hemifumarate). Background technique [0002] Tenofovir alafenamide (tenofovir alafenamide), the chemical name is 9-[(R)-2-[[(S)-1-(isopropoxycarbonyl)ethyl]aminophenoxyphosphinyl ]Methoxyl]propyl]adenine] is a new type of nucleotide reverse transcriptase inhibitor developed by Gilead Sciences of the United States. Launched in the United States in 2015, it is used to treat HIV infection in adults and is also used to treat hepatitis B. Tenofovir alafenamide hemifumarate is a drug used to inhibit hepatitis B virus developed by Gilead in the United States. It was approved by the FDA in November 2017. The trade name is Vemlidy. Treatment of patients with chronic hepatitis B infection with compensated liver disease, as a nucleoside reverse transcriptase inhibitor, it is a prodrug of tenofovir, compared with tenofov...

Claims

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Application Information

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IPC IPC(8): C07F9/6561
CPCC07B2200/13C07F9/65616
Inventor 唐云何帅洁卓国清黄浩喜李英富苏忠海
Owner CHENGDU BRILLIANT PHARMA CO LTD
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