Preparing apabetalone and its polymorphs used for treating atherosclerosis, involves stirring charged dimethylacetamide, 4-(2-hydroxyethoxy)-3,5-dimethylbenzaldehyde, 2-amino-3,5-dimethoxybenzamide and p-Toluenesulfonic acid, crystallizing the DMAc solvated material in n-propanol and water
	TIWARI K I; KATESHAM R V; RACHAKONDA S
	2024-04-23
专利权人	TYLON PHARMA LTD (TYLO-Non-standard) ; TYLON PHARMA PTE LTD (TYLO-Non-standard) ; VCS CHEM TECH PVT LTD (VCSC-Non-standard)
申请日期	2024-04-23
专利号	IN202441032013-A
成果简介	NOVELTY - Preparing apabetalone and its polymorphs, involves: (A) preparing DMAc solvated material via (i) stirring charged dimethylacetamide (DMAc), 4-(2-hydroxyethoxy)-3,5-dimethylbenzaldehyde, 2-amino-3,5-dimethoxybenzamide and p-Toluenesulfonic acid monohydrate; (ii) adding charged sodium bisulfite Lot-01 to the reaction mass and heating to 115-120℃ and maintaining for 90-105 minutes; (B) crystallizing DMAc solvated material in n-propanol via (i) heating charged DMAc solvated material, n-propanol and activated charcoal followed by stirring for 3-4 hours to get 2.0 g apabetalone; and (C) crystallizing DMAc solvated material in mixture of n-propanol and water via (i) heating charged DMAc solvated material, 30.0 mL n-propanol and activated charcoal followed by filtering under reduced pressure, washing with n-propanol; (ii) transferring the filtrate into 4 Normal round bottom flask (RBF) and heating to 40-45℃ to get 2.0 g apabetalone. USE - Process for preparing apabetalone and its polymorphs used for treating atherosclerosis and associated cardiovascular disease. No biological data given. ADVANTAGE - The process is simple, convenient, safe and scalable with low pricing, and utilize non-hazardous and easy to operate raw materials or catalyst or reagents. DETAILED DESCRIPTION - Preparing apabetalone and its polymorphs, involves: (A) preparing DMAc solvated material via (i) stirring charged 10.0 g DMAc, 2.1 g 4-(2-hydroxyethoxy)-3,5-dimethylbenzaldehyde, 2.0 g 2-amino-3,5-dimethoxybenzamide and p-TSA.H2O; (ii) adding 0.86 g charged sodium bisulfite Lot-01 to the reaction mass and heating to 115-120℃ and maintaining for 90-105 minutes, then again adding 0.86 g sodium bisulfite Lot-02 and maintaining for 90-105 minutes, and after that, adding 0.86 g sodium bisulfite Lot-03 and maintaining for overnight to get DMAc solvated material; (B) crystallizing DMAc solvated material in n-propanol via (i) heating charged DMAc solvated material, 30.0 mL n-propanol and activated charcoal, filtering under reduced pressure, washing with n-propanol, cooling to ambient temperature and stirring for 3-4 hours to get the solid formation; and (ii) filtering the solid under reduced pressure, washing with n-propanol, and drying the wet material at 60-65℃ to get 2.0 g apabetalone, where apabetalone is characterized by powder X-ray diffraction (PXRD) (2θ): 6.002, 7.324, 8.527, 9.046, 11.252, 11.971, 12.863, 16.190, 20.362, 23.201, 25.012, 26.006, 26.722±0.1, and DSC data as shown in the table; and (C) crystallizing DMAc solvated material in mixture of n-propanol and water via (i) heating charged DMAc solvated material, 30.0 mL n-propanol and activated charcoal followed by filtering under reduced pressure, washing with n-propanol; (ii) transferring the filtrate into 4 Normal RBF and heating to 40-45℃ to get the clear solution; (iii) charging 30.0 mL water at 40-45℃ and maintaining for 3-40 minutes, then cooling the mass to ambient temperature and stirring for 3-4 hours to get the solid formation; and (iii) filtering the solid under reduced pressure, washing with n-propanol and drying the wet material at 60-65℃ to get the 2.0 g apabetalone, where the apabetalone is characterized by PXRD (2θ): 6.078, 8.609, 11.413, 12.066, 12.671, 12.969, 14.043, 16.287, 18.454, 20.051, 20.445, 23.170, 23.371, 24.232, 25.089, 26.110, 26.835, and DSC data as shown in the table.
IPC 分类号	A61K-031/517 ; A61P-003/12 ; C07D-239/91 ; C07D-403/04 ; C07D-403/12
国家	印度
专业领域	医药卫生
语种	英语
成果类型	专利
文献类型	科技成果
条目标识符	http://119.78.100.226:8889/handle/3KE4DYBR/17027
专题	中国科学院新疆生态与地理研究所
作者单位	1.TYLON PHARMA LTD (TYLO-Non-standard) 2.TYLON PHARMA PTE LTD (TYLO-Non-standard) 3.VCS CHEM TECH PVT LTD (VCSC-Non-standard)
推荐引用方式 GB/T 7714	TIWARI K I,KATESHAM R V,RACHAKONDA S. Preparing apabetalone and its polymorphs used for treating atherosclerosis, involves stirring charged dimethylacetamide, 4-(2-hydroxyethoxy)-3,5-dimethylbenzaldehyde, 2-amino-3,5-dimethoxybenzamide and p-Toluenesulfonic acid, crystallizing the DMAc solvated material in n-propanol and water. IN202441032013-A[P]. 2024.

条目包含的文件
条目无相关文件。

除非特别说明，本系统中所有内容都受版权保护，并保留所有权利。