Crystalline polymorph of pipindoxifene hydrochloride monohydrate
A polymorph, monohydrate technology, applied in the field of selective estrogen receptor modulators
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0033] Examples of the preparation of Forms I and II are provided in the Examples. Generally, the polymorph product is released from the solvent by dissolving piridoxifene hydrochloride (any form, including amorphous) in a suitable aqueous solvent and by any conventional method known in the art, such as cooling or evaporating the solvent. Crystallization, Form I can be prepared. Suitable solvents include mixtures of water, alcohols and optionally ethers. The water content of the solvent appeared to affect the relative amounts of Form I and Form II that precipitated. A higher content of water in the solvent favors Form II while a low content of water favors Form I.
[0034] In the preparation of Form II, the volume ratio of water to alcohol in the crystallization solvent may be greater than about 1:5. In some embodiments, the volume ratio of water to alcohol in the preparation of Form II is about 2 to about 1:5, about 1 to about 1:5, about 1:2 to about 1:5, about 2:5 to abo...
Embodiment 1
[0062] Preparation of piridoxifene hydrochloride monohydrate crystal form I
[0063] Into a 1 L three-necked flask equipped with a mechanical stirrer, temperature probe, reflux condenser and nitrogen atmosphere were charged 150 g of piridoxifene hydrochloride, 1035 g, 1312 mL of pre-filtered ethanol and 188 g of purified water. The mixture was heated to 78-80°C over a minimum of 45 minutes to form a solution. The resulting solution was stirred at moderate speed at 80°C for 15 minutes. The stirring speed was reduced to 75 rpm and the solution was allowed to cool to 22-25°C within 5 hours. Crystallization started at 65-67°C. The slurry was maintained at 22-25°C for at least 1 hour before solids were collected by filtration on a 12.5 cm Buchner funnel with filter paper. The filter cake was washed with ethanol (118 g / 150 mL, pre-filtered and pre-cooled to 10-15 °C). The filter cake was then drained until dripping ceased, at which point it had a depth of 1.6 cm. The filter cak...
Embodiment 2
[0065] Method for preparing piridoxifene hydrochloride monohydrate crystal form II from crystal form I
[0066] Into a 1 L three-necked flask equipped with a mechanical stirrer, temperature probe, reflux condenser and nitrogen atmosphere, 20 g of a sample of piridoxifene hydrochloride Form I, 280 mL of ethanol and 120 mL of purified water were added. The material introduced into the flask showed a DSC peak at 188°C, indicating Form I. The mixture was heated to reflux temperature to dissolve the piridoxifene. The mixture was cooled to 22°C over 3 hours and a visible slurry formed. The mixture was filtered and the precipitate was washed with 20 mL of cold ethanol. The product was dried in a vacuum oven at 40° C. for 2 hours and then at room temperature for a further 22 hours. DSC scan revealed a new polymorph (Form II) with a peak at 179°C. See Example 6 for the DSC method. The product yield was 74%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More - R&D
- Intellectual Property
- Life Sciences
- Materials
- Tech Scout
- Unparalleled Data Quality
- Higher Quality Content
- 60% Fewer Hallucinations
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com