Preparing crystalline Form II of triaminopyrimidine derivative used for treating malaria, involves crystallizing triaminopyrimidine derivative from solvents, e.g., ethyl acetate, or mixture of two solvents, where one is acetonitrile, and other solvent is dichloromethane, ethyl acetate, chloroform
	GAJJAR S R; LALPARA J N; GHODASARA H B; KALAVADIYA P L; PATIL A K; SINGH N A; RATHORE K; SINGH K K
	2023-08-22
专利权人	ZYDUS LIFESCI LTD (CDLA-C)
申请日期	2023-08-22
专利号	IN202321056118-A
成果简介	NOVELTY - Preparing crystalline Form II of triaminopyrimidine derivative of formula (I), involves: crystallizing triaminopyrimidine derivative (I) from one or more solvents selected from: ethyl acetate, dichloromethane, chloroform; or a mixture of two solvents, where one of the solvent is acetonitrile, and other is dichloromethane, ethyl acetate, and chloroform, where crystalline Form II of triaminopyrimidine derivative is characterized by X-ray powder diffraction pattern having peaks in 2θ at 13.8°, 21.9°, and 23.7°±0.2°; or (a) heating a mixture of triaminopyrimidine derivative (I) and solvents; and (b) cooling the solution to obtain the crystalline Form II of triaminopyrimidine derivative (I); or (c) reacting pyrimidine derivative of formula (II) of with formaldehyde in the presence of a suitable reducing agent in dichloromethane at 25-35℃ to obtain a reaction mixture; (d) adding water to the reaction mixture; (c) basifying the reaction mixture. USE - Preparing crystalline Form II of triaminopyrimidine derivative used for preventing or treating malaria. No biological data given. ADVANTAGE - The process is robust, scalable and reproducible. DETAILED DESCRIPTION - Preparing crystalline Form II of triaminopyrimidine derivative of formula (I), involves: crystallizing triaminopyrimidine derivative (I) from one or more solvents selected from: ethyl acetate, dichloromethane, chloroform, or a mixture; or a mixture of two solvents, where one of the solvent is acetonitrile, and other solvent is selected from dichloromethane, ethyl acetate, and chloroform, where crystalline Form II of triaminopyrimidine derivative is characterized by X-ray powder diffraction pattern having peaks in 2θ at 13.8°, 21.9°, and 23.7°±0.2°; or (a) heating a mixture of triaminopyrimidine derivative (I) and solvents to obtain a solution; and (b) cooling the solution to obtain the crystalline Form II of triaminopyrimidine derivative (I); or (c) reacting pyrimidine derivative of formula (II) of with formaldehyde in the presence of a suitable reducing agent in dichloromethane at 25-35℃ to obtain a reaction mixture; (d) adding water to the reaction mixture; (c) basifying the reaction mixture; (e) separating the organic layer and concentrating under reduced pressure to obtain a residue; (f) adding a mixture of acetonitrile and dichloromethane to the residue to obtain a reaction mixture; (g) heating the reaction mixture at 70-85℃ to obtain a solution; (h) cooling the solution to 60-68℃, and seeding with the crystalline Form II of triaminopyrimidine derivative (I); (i) cooling to 5-35℃; and (j) obtaining the crystalline Form II of triaminopyrimidine derivative (I); or (A) heating a mixture of triaminopyrimidine derivative (I) and 5-20 mL solvents at 50-90℃, for 15 minutes to 2 hours to obtain a solution; (B) cooling the solution at 5-35℃ to obtain a suspension; (C) stirring the suspension at 5-35℃ for 20 minutes to 2 hours; and (D) obtaining the crystalline Form II of triaminopyrimidine derivative (I).
IPC 分类号	C07D-401/14
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/20737
专题	中国科学院新疆生态与地理研究所
作者单位	ZYDUS LIFESCI LTD (CDLA-C)
推荐引用方式 GB/T 7714	GAJJAR S R,LALPARA J N,GHODASARA H B,et al. Preparing crystalline Form II of triaminopyrimidine derivative used for treating malaria, involves crystallizing triaminopyrimidine derivative from solvents, e.g., ethyl acetate, or mixture of two solvents, where one is acetonitrile, and other solvent is dichloromethane, ethyl acetate, chloroform. IN202321056118-A[P]. 2023.

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