Crystalline form of (s)-(2-(6-chloro-7-methyl-1h-benzo[d]imidazol-2-yl)-2-methylpyrrolidin-1 -yl)(5-methoxy-2-(2h-1,2,3-triazol-2-yl)phenyl)methanone and its use as orexin receptor antagonists
A kind of methylpyrrolidine, methoxyl technology, applied in (S)-(2-(6-chloro-7-methyl-1H-benzo[d]imidazol-2-yl)-2-methyl Crystalline form of pyrrolidin-1-yl)(5-methoxy-2-(2H-1,2,3-triazol-2-yl)phenyl)methanone and its use as orexin receptor antagonist It can solve problems such as prevention and effective treatment that have not yet appeared
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0159] Preparative HPLC for Purification of Compounds (Condition C)
[0160] Column: WatersXBridge (10 μm, 75×30 mm). Conditions: MeCN [eluent A]; water + 0.5% NH 4 OH (25% aq.) [eluent B]; Gradient: 90% B→5% B over 6.5 min. (Flow rate: 75ml / min). Detection: UV+ELSD.
[0161] Preparative HPLC for Purification of Compounds (Condition D)
[0162] Column: Waters Atlantis T3OBD (10 μm, 75×30 mm). Conditions: MeCN [eluent A]; water + 0.5% HCOOH [eluent B]; gradient: 90% B→5% B over 6.4 min. (Flow rate: 75ml / min). Detection: UV+ELSD.
[0163] LC-MS under acidic conditions
[0164] Device: Agilent 1100 series with mass spectrometry detection (MS: Finnigan single quadrupole). Column: Agilent Zorbax SB-Aq, (3.5 μm, 4.6×50mm). Conditions: MeCN [eluent A]; water+0.04% TFA [eluent B]. Gradient: 95% B → 5% B over 1.5 min. (Flow rate: 4.5ml / min). Detection: UV+MS.
[0165] X-ray powder diffraction (XRPD) analysis
[0166] In having the CuK a - X-ray powder diffraction patter...
example 1
[0195] Example 1: Preparation and Characterization of Compounds in Form 1
[0196] a) Preparation of Seed Material of Compound in Form 1
[0197] In a 7 mL vial, 0.2 g of the compound as an amorphous mass was dissolved in 2 mL of MeOH. Samples were left open at ambient and evaporated over the weekend. Amorphous lumps with some crystals were obtained as observed under crossed polarizers. 0.05 mL of MeOH was added, the vial was closed and the sample was sonicated for 1 min and heated to 40°C. This procedure was repeated 3 to 4 times to cause further crystallization and after about 15 min the sample was further shaken at 25°C for 1 h. Thereafter the solid was isolated, dried under reduced pressure (2 mbar, room temperature) for 4 hours and allowed to equilibrate open at room temperature and 58% relative humidity for 2 hours. An off-white powder was obtained as the compound in Form 1. It may be necessary to repeat this procedure several times to obtain sufficient material for...
example 2
[0203] Example 2: Preparation and Characterization of Compounds in Form 2
[0204] 0.05 mL of acetonitrile was mixed with 0.01 g of the compound in Form 1 in a 4 mL glass with a magnetic stirrer for 3 days at room temperature. The solid was isolated and dried under reduced pressure (2 mbar for 30 min) and was the compound in Form 2.
[0205] Alternatively, 0.1 mL of methyl-isobutyl ketone was mixed with 0.015 g of the compound in Form 1 in a 4 mL glass with a magnetic stirrer for up to 3 days at room temperature. The solid was isolated and dried under reduced pressure (2 h at 2 mbar) and was the compound in Form 2.
[0206] Table 3: Characterization data for the compound in Form 2
[0207]
[0208] III. Bioanalysis
PUM
Property | Measurement | Unit |
---|---|---|
melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
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