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82626-48-0Relevant articles and documents
Structural and thermal characterization of zolpidem hemitartrate hemihydrate (Form E) and its decomposition products by laboratory x-ray powder diffraction
Halasz, Ivan,Dinnebier, Robert E.
, p. 871 - 878 (2010)
The crystal structure of zolpidem hemitartrate hemihydrate (I, Form E) has been solved from high-resolution laboratory powder diffraction data. It crystallizes in the orthorhombic P212121 space group with a=22.4664(6)?, b=26.0420(7)?, and c=7.4391(1)?. Protonation of zolpidem molecules could not be unambiguously determined. Thermal stability of Form E has been investigated by TG-DTA and in situ by temperature resolved X-ray powder diffraction. Water loss occurs between 508C≤t≤1008C while structure decomposition commences at approximately 120°C yielding zolpidem tartrate (II) and pure zolpidem base (III) in approximately equimolar amounts. Crystal structures of II and III have been solved simultaneously from a single powder pattern of thermally decomposed I. Zolpidem tartrate crystallizes in the orthorhombic P212121 space group with a=19.9278(8)?, b=15.1345(8)?, and c=7.6246(2)? (at 140°C). Zolpidem base crystallizes in the orthorhombic Pcab space group with a=9.9296(4)?, b=18.4412(9)?, and c=18.6807(9)? (at 140°C). In the reported crystal structures zolpidem molecules form stacks through π-π interaction or dipole-dipole interactions while tartrate moieties, if present, form hydrogen bonded chains. Water molecule in I forms a hydrogen bond to the imidazole nitrogen atom of the zolpidem molecule. Free space in the crystal structure of I could allow for the additional water molecules and thus a variable water content.
An improved and scalable synthesis of zolpidem via a CuI/BINOL-mediated tandem reaction of imine and alkyne
Zhang, Bingbing,Shan, Guangsheng,Ma, Qiaoning,Xu, Qianqian,Lei, Xinsheng
, p. 445 - 448 (2017)
An improved and scalable method for the synthesis of zolpidem (1), a hypnotic drug, was developed. A two-step sequence involving imine formation and subsequent tandem reaction between an imine and propiolamide in the presence of CuI/BINOL, an efficient promoter for the tandem reaction, is described. Zolpidem was efficiently prepared in a 54% isolated yield and the hemitartrate salt of zolpidem was produced in 37% yield by simple crystallization, without tedious column chromatography. The procedure can be scaled up to >10 g. The yield of 1 increased to 83% following isolation of the intermediate imine 5.
Zolpidem preparation method
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Paragraph 0046-0067, (2022/02/24)
The invention belongs to the technical field of drug synthesis, and provides a zolpidem preparation method which comprises the following steps: by taking SM-1 as a starting material, Rh (trop2N) (PPh3) as a catalyst and MMA as a hydrogen acceptor, carrying out catalytic dehydrogenation coupling reaction on the starting material, the catalyst and dimethylamine, and carrying out acid dissolution and alkali precipitation refining to obtain a product with higher purity. Compared with the prior art, the zolpidem preparation process has the advantages that the process route can be obviously shortened, and the preparation process is suitable for industrial production.
Synthesis of C3-Cyanomethylated Imidazo[1,2- a ]pyridines via Ultrasound-Promoted Three-Component Reaction under Catalyst- and Oxidant-Free Conditions
Wu, Qingguo,Yang, Haifeng,Zhang, Jian,Zhang, Jie,Zhang, Yufeng
, p. 264 - 268 (2022/02/05)
An efficient synthesis of C3-cyanomethylated imidazo[1,2-α]pyridines via ultrasound-promoted three-component reaction under catalyst-free, oxidant-free, and mild conditions has been developed. A series of C3-cyanomethylated imidazo[1,2-α]pyridines were rapidly prepared with satisfactory yields and good functional group compatibility. This strategy cloud also be applied to the synthesis of zolpidem and alpidem in short steps.
One-Pot Synthesis of C3-Alkylated Imidazopyridines from α-Bromocarbonyls under Photoredox Conditions
Li, Jingyu,Liu, Ping,Sun, Peipei,Tong, Jinwen,Zhan, Yanling
supporting information, p. 4541 - 4545 (2021/08/27)
A convenient strategy is presented for the synthesis of C3-alkylated imidazopyridines through one pot condensation and alkylation of α-bromocarbonyl compounds with 2-aminopyridines. A series of C3-alkylated imidazopyridines were obtained in moderate to hi
Preparation method of zolpidem
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Paragraph 0021; 0077-0086, (2021/08/19)
The invention discloses a preparation method of a zolpidem intermediate. In the process of preparing the zolpidem intermediate N, N, 6-trimethyl-2-(4-methylphenyl)-imidazo [1, 2-alpha] pyridine-3-acetamide hydrochloride by reducing N, N, 6-trimethyl-2-(4-methylphenyl)-imidazo [1, 2-alpha] pyridine-3-acetamide hydrochloride, through process optimization and parameter adjustment, by using a 10% palladium-carbon catalyst and combining the reaction condition of hydrogen pressure of 0.02-0.09 MPa, the conversion effect of the N, N, 6-trimethyl-2-(4-methylphenyl)-imidazo [1, 2-alpha] pyridine-3-chloroacetamide hydrochloride is promoted, side reactions and impurities are reduced, the product yield is increased, the problem of low product synthesis yield in the process of preparing N, N, 6-trimethyl-2-(4-methylphenyl)-imidazo [1, 2-alpha] pyridine-3-acetamide hydrochloride through reduction reaction in zolpidem production is solved, and the production cost of zolpidem tartrate is reduced.
Preparation method of zolpidem
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Paragraph 0043; 0049; 0050, (2020/05/05)
The invention belongs to the field of pharmacy, and relates to a method for preparing zolpidem. The preparation method comprises the following steps: taking maleic anhydride and 2-amino-4-methylpyridine as raw materials, and carrying out a series of react
Study on a three-step rapid assembly of zolpidem and its fluorinated analogues employing microwave-assisted chemistry
Fajkis, Nikola,Gryzlo, Beata,Kolaczkowski, Marcin,Krupa, Anna,Marcinkowska, Monika
, (2020/08/24)
We developed an efficient microwave-assisted three-step synthesis of zolpidem and its fluorinated analogues 1-3. The procedure relays on the utilization of easily accessible and inexpensive starting materials. Our protocol shows superior performance in terms of yield and purity of products, compared to conventional heating systems. Notably, the total time needed for reaction accomplishment is significantly lower comparing to oil bath heating systems. Finally, we have performed a detailed study on the preparation of zolpidem tartrate salt I, and we assessed its particle-sizes using a polarizing microscope. Our goal was to select the appropriate method that generates the acceptable particle-size, since the solid-size directly influences solubility in biological fluids and further bioavailability. We believe that the disclosed procedure will help to produce a lab-scale quantity of zolpidem and its fluorinated derivatives 1-3, as well as zolpidem tartrate salt I, with suitable fine-particle size for further biological experimentation.
Rhodium catalyzed direct C3-ethoxycarbonylmethylation of imidazo[1,2-a]pyridines with ethyl diazoacetate
Dong, Hui,Hu, Wenhao,Huang, Qiuyao,Li, Bingbing,Wang, Yuanxiang
supporting information, (2020/02/13)
An efficient and environment-friendly C3-ethoxycarbonylmethylation of imidazo[1,2-a]pyridines with ethyl diazoacetate in the presence of a Rh(II) catalyst was developed. Such strategy not only enables the synthesis of zolpidem, but also provides a way to
Practical and scalable preparation of Minodronic acid and Zolpidem from 2-chloroimidazole[1,2-a]pyridines
Wang, Yuheng,Zhang, Bingbing,Zheng, Yinying,Ma, Qiaoning,Sui, Qiang,Lei, Xinsheng
, p. 1064 - 1071 (2019/01/14)
Practical and scalable procedures for Minodronic acid and Zolpidem are developed with short reaction sequences from 2-aminopyridines and maleic anhydride, respectively. The new procedures avoid column chromatography for the purification in all synthetic steps. Key aspects of this development involve reductive hydrodechlorination and Suzuki coupling reaction of 2-chloroimidazole[1,2-a]pyridines, and their application towards synthesis of the two drugs is also addressed.