Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Vilazodone hydrochloride crystal form and preparation method thereof

A vilazodone hydrochloride crystal form and a technology for vilazodone hydrochloride are applied in the field of new vilazodone hydrochloride crystal form A and its preparation, and can solve the problems of low rate of defective products in tablets and the like

Active Publication Date: 2016-08-03
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
View PDF7 Cites 2 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Vilazodone hydrochloride crystal form and preparation method thereof
  • Vilazodone hydrochloride crystal form and preparation method thereof
  • 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]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
melting pointaaaaaaaaaa
strengthaaaaaaaaaa
Login to View More

Abstract

The invention relates to a vilazodone hydrochloride crystal form. The powder X-ray powder diffraction pattern of the crystal form has characteristic peaks when a diffraction angle 2theta is 9.019+ / -0.2 DEG, 14.481+ / -0.2 DEG, 18.839+ / -0.2 DEG, and 24.580+ / -0.2 DEG, 27.271+ / -0.2 DEG, the relative intensity of the diffraction angle 2theta at 24.580+ / -0.2 DEG is 100%, the relative intensity of the diffraction angle 2theta at 18.839+ / -0.2 DEG is no less than 70%, the relative intensity of the diffraction angle 2theta at 14.481+ / -0.2 DEG is no less than 30%, the relative intensity of the diffraction angle 2theta at 9.019+ / -0.2 DEG is no less than 20%, and the relative intensity of the diffraction angle 2theta at 27.271+ / -0.2 DEG is no less than 18%. The invention also relates to a preparation method of the vilazodone hydrochloride crystal form, a pharmaceutical composition and the vilazodone hydrochloride crystal form in preparation of medicine for treating depression.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com