A kind of vilazodone hydrochloride crystal form and preparation method thereof

A technology of vilazodone hydrochloride and crystal form, which is applied in the field of vilazodone hydrochloride new crystal form A and its preparation, can solve the problem of low defective product rate in tablet forming, and achieve low defective product rate and high yield High, uniform effect

Active Publication Date: 2021-05-25
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, there are still some fluidity and fragmentation problems in IV crystallization. Therefore, it is still necessary to further study the crystal form of vilazodone hydrochloride to find a crystal form with better fluidity, low tablet defect rate, and more suitable The new crystal form of industrial production is an extremely important work in the drug research of vilazodone hydrochloride

Method used

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  • A kind of vilazodone hydrochloride crystal form and preparation method thereof
  • A kind of vilazodone hydrochloride crystal form and preparation method thereof
  • A kind of vilazodone hydrochloride crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Embodiment 1: Preparation of vilazodone hydrochloride crystal form A

[0069] ①Under room temperature, dissolve vilazodone powder (12g, 27.2mmol) in THF (tetrahydrofuran) (240mL), slowly add water (480mL) into the solution under stirring, after the addition is complete, stir at room temperature for 30min;

[0070] ② Add 2M hydrochloric acid aqueous solution (24.5mL, 49mmol) to the solution system, cool down to 10°C, stir for 2-3h, and crystallize;

[0071] ③ suction filtration, filter cake water (48mL) rinse;

[0072] ④ The obtained solid is then vacuum-dried at 50°C-60°C (vacuum degree ≥ 0.09MPa), and dried for 2h to obtain vilazodone hydrochloride crystal form A of the present invention (11.5g, yield 88.5%, purity (HPLC detection) is 99.78%).

[0073] Measure the vilazodone hydrochloride crystal form A obtained in step 4., as follows:

[0074] (1) Powder X-ray Diffraction Measurement Results

[0075] The powder X-ray diffraction pattern of table 1 vilazodone hydro...

Embodiment 2-4

[0084] Example 2-4: Preparation of vilazodone hydrochloride crystal form A

[0085] With reference to the preparation process of Example 1, the consumption of purified water in step 2. is changed to 528mL, 600mL, 720mL respectively, that is, the water (H 2 O) and the volume ratio of tetrahydrofuran in step ① (see Table 3 below for details), respectively, to obtain vilazodone hydrochloride crystal form A of the present invention.

[0086] Table 3 water and tetrahydrofuran volume ratio investigation result

[0087]

Embodiment 5～6

[0093] Embodiments 5-6: Preparation of vilazodone hydrochloride crystal form A

[0094] With reference to the preparation process of Example 1, only the volume of the 2M hydrochloric acid added in step ② was changed to 20.4mL (40.8mmol) and 27.2mL (54.4mmol) respectively, that is, the volume ratio of hydrochloric acid in step ② to tetrahydrofuran in step ① was changed The obtained vilazodone hydrochloride yield and purity (HPLC detection) of the present invention are specifically shown in Table 5 below.

[0095] Table 5 hydrochloric acid addition investigation result

[0096]

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Abstract

The present invention relates to a new crystal form of vilazodone hydrochloride. The 2θ angles of the crystal form on the powder X-ray diffraction pattern are 9.019±0.2°, 14.481±0.2°, 18.839±0.2°, 24.580±0.2°, There is a characteristic peak at 27.271±0.2°, and the relative intensity of the characteristic peak at the 2θ angle of 24.580±0.2° is 100%, the relative intensity of the characteristic peak at the 2θ angle of 18.839±0.2° is not less than 70%, and the 2θ angle is at 14.481±0.2 The relative intensity of the characteristic peak at ° is not less than 30%, the relative intensity of the characteristic peak at the 2θ angle of 9.019±0.2° is not less than 20%, and the relative intensity of the characteristic peak at the 2θ angle of 27.271±0.2° is not less than 18%. The invention also relates to a preparation method, a pharmaceutical composition and a medicine for treating depression of the vilazodone hydrochloride crystal form.

Description

technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a new crystal form A of vilazodone hydrochloride and a preparation method thereof. Background technique [0002] Vilazodone (Vilazodone), trade name Viibryd, the US Food and Drug Administration (FDA) approved in July 2011, the chemical name is 1-[4-(5-cyanindol-3-yl) butyl ]-4-(2-carbamoyl-benzofuran-5-yl)-piperazine, its structural formula is as shown in formula 1: [0003] [0004] Vilazodone is an antidepressant drug with dual effects, which belongs to selective 5-HT reuptake inhibitors (SSRIs) and 5-HT1A partial agonists. Rapidly increase the extracellular concentration of 5-HT to exert a rapid antidepressant effect. It is the first drug in the new class of indolealkylamine antidepressants and the first new antidepressant to be obtained by pharmacogenomic screening. The drug is effective, well tolerated, and rapidly effective in the treatment of depression...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D405/12A61K31/496A61P25/24
Inventor 杨占坤郭晓伟张琪齐珊郑利刚张倩如郭明东
Owner CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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