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Rilpivirine hydrochloride alcoholate polymorph and preparation method thereof

A technology of warin hydrochloride and polymorphs, applied in the field of rilpivirine hydrochloride alcoholate polymorphs and its preparation, can solve the problem of easy damage to drying equipment, difficult drying of crystallization, and corrosion of acetic acid sexual issues

Active Publication Date: 2016-04-27
江西迪赛诺制药有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The crystals obtained by this method are not easy to dry, and acetic acid is corrosive, and the drying equipment is easily damaged, so it is not suitable for industrial production

Method used

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  • Rilpivirine hydrochloride alcoholate polymorph and preparation method thereof
  • Rilpivirine hydrochloride alcoholate polymorph and preparation method thereof
  • Rilpivirine hydrochloride alcoholate polymorph and preparation method thereof

Examples

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preparation example Construction

[0124] One, the present invention provides a kind of new preparation method of preferably rilpivirine hydrochloride type C polymorph, comprising steps:

[0125] (c1) dissolving rilpivirine hydrochloride in an inert solvent to obtain a rilpivirine hydrochloride solution;

[0126] (c2) cooling (such as down to 0 ~ 10 ℃), crystallization;

[0127] (c3) filtering to obtain the C-type polymorph of rilpivirine hydrochloride;

[0128] Wherein, the inert solvent is selected from the group consisting of N-methyl-2-pyrrolidone, dimethylsulfoxide, formamide, N,N-dimethylformamide or combinations thereof.

[0129] In another preferred example, the inert solvent is N-methyl-2-pyrrolidone.

[0130] In another preferred example, the rilpivirine hydrochloride may be a polymorph of rilpivirine hydrochloride or an alcoholate polymorph of rilpivirine hydrochloride; preferably non-C Type rilpivirine hydrochloride polymorph, such as type A rilpivirine hydrochloride, type E polymorph according t...

Embodiment 1

[0150] Preparation of Rilpivirine Hydrochloride Methanolate Type E Polymorph

[0151] Add 5 g of rilpivirine hydrochloride into 25 mL of anhydrous methanol, stir at 25° C. for 6 hours, filter, collect the solid, and dry to obtain a polymorph of rilpivirine hydrochloride methanolate type E.

Embodiment 2

[0153] Preparation of Rilpivirine Hydrochloride Methanolate Type E Polymorph

[0154] Add 5 g of rilpivirine hydrochloride into 25 mL of anhydrous methanol, raise the temperature to reflux, stir for 2 hours, filter, collect the solid, and dry to obtain rilpivirine hydrochloride methanolate type E polymorph.

[0155] For the crystals of rilpivirine hydrochloride methanolate prepared in Example 1-2, it was confirmed by X-ray powder diffraction and thermogravimetric analysis that the obtained crystals were all E-type polymorphs. Its powder X-ray diffraction pattern is as figure 1 As shown, the thermogravimetric analysis spectrum is as figure 2 shown.

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Abstract

The invention relates to rilpivrine hydrochloride alcoholate polymorphs and preparation methods thereof. Specifically, the invention discloses the following three rilpivrine hydrochloride alcoholates polymorphs and preparation methods thereof: rilpivrine hydrochloride methanolate E-type polymorph, rilpivrine hydrochloride ethanolate F-type polymorph, and rilpivrine hydrochloride n-propanolate G-type polymorph. The invention also discloses a novel preparation method of rilpivrine hydrochloride A-type or C-type polymorphs.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a rilpivirine hydrochloride alcoholate polymorph and a preparation method thereof. Background technique [0002] Rilpivirine hydrochloride (trade name EDURANT) is an HIV non-nucleoside reverse transcriptase inhibitor developed by Tibotec, a subsidiary of Johnson & Johnson. This product is a new type of diarylpyrimidine drug with strong antiviral activity, high oral bioavailability, good safety, and will not induce any changes in virus genotype or genotype. Its structural formula is as follows: [0003] [0004] In the prior art, reports on polymorphs of rilpivirine hydrochloride have also appeared. For example, WO2006024668A1 discloses type A, type B, type C and type D polymorphs of rilpivirine hydrochloride. Rilpivirine hydrochloride type A crystal is currently used clinically. WO2006024668A1 reports the preparation method of crystal form A: dissolv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/48
Inventor 李金亮赵楠胡文军周春峰赵海鲲李海峰
Owner 江西迪赛诺制药有限公司