557-30-2Relevant articles and documents
Preparation, crystal structure and properties of a new crystal form of diammonium 5,5′-bistetrazole-1,1′-diolate
Wang, Xiaojun,Jin, Shaohua,Zhang, Chunyuan,Li, Lijie,Chen, Shusen,Shu, Qinghai
, p. 1229 - 1234 (2015)
A new crystal form of diammonium 5,5′-bistetrazole-1,1′-diolate (1) was prepared by two novel methods and fully characterized by using IR, NMR spectroscopy, elementary analysis, single crystal X-ray crystallography and thermal gravity/differential thermal analysis (TG/DTA). Crystalline 1 was found as monoclinic and space group of P21/c (14). The TG/DTA analysis showed that the decomposition temperature of 1 was 287.8°C with a mass loss of 91.2% in the range of 220-300°C at a heating rate of 5°C/min. The sensitivities test towards impact, friction of 1 indicated that 1 has much lower sensitivities than those of RDX/HMX and is comparable to those of TNT, which suggested that 1 could be used as a good candidate of new insensitive energetic compound. A new crystal form of diammonium 5,5′-bistetrazole-1,1′-diolate (1) was prepared by two different novel methods and found as monoclinic and space group of P21/c (14). The thermal decomposition analysis and sensitivities test towards impact, friction of 1 indicated that 1 has much lower sensitivities than those of RDX/HMX and comparable to those of TNT, which suggested that 1 could be used as a good candidate of new insensitive energetic compound.
Method for preparation of insensitive high explosive
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Page/Page column 7, (2021/11/03)
The present invention provides a method for the preparation of an insensitive high enthalpy explosive Dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate (TKX-50) in the presence of N,N-dimethylformamide, N,N-dimethylacetamide, or N-Methyl-2-pyrrolidone as a solvent via a four-step, one-pot reaction route to obtain a final product after four reaction steps. The more dangerous intermediate diazidoglyoxime may be solved by the one-pot method without the need of isolation. Further, the cyclization reaction is carried out in the presence of dropwisely added concentrated sulfuric acid to replace hydrochloric gas so no hydrochloric gas generator is needed to greatly reduce the amount of waste acid so as to effectively reduce the cost by avoiding using hydrochloric gas steel cylinders which require much safety equipment.
High-Throughput Screening of Earth-Abundant Water Reduction Catalysts toward Photocatalytic Hydrogen Evolution
Motz, Rachel N.,Lopato, Eric M.,Connell, Timothy U.,Bernhard, Stefan
supporting information, p. 774 - 781 (2021/02/05)
Noble-metal photosensitizers and water reduction co-catalysts (WRCs) still present the highest activity in homogeneous photocatalytic hydrogen production. The search for earth-abundant alternatives is usually limited by the time required to screen new catalyst combinations; however, here, we utilize newly designed and developed high-throughput photoreactors for the parallel synthesis of novel WRCs and colorimetric screening of hydrogen evolution. This unique approach allowed rapid optimization of photocatalytic water reduction using the organic photosensitizer Eosin Y and the archetypal cobaloxime WRC [Co(GL1)2pyCl], where GL1 is dimethylglyoxime and py is pyridine. Subsequent combinatorial synthesis generated 646 unique cobalt complexes of the type [Co(LL)2pyCl], where LL is a bidentate ligand, that identified promising new WRC candidates for hydrogen production. Density functional theory (DFT) calculations performed on such cobaloxime derivative complexes demonstrated that reactivity depends on hydride affinity. Alkyl-substituted glyoximes were necessary for hydrogen production and showed increased activity when paired with ligands containing strong hydrogen-bond donors.
METHOD FOR SYNTHESIS OF TKX-50 USING INSENSITIVE INTERMEDIATE
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Paragraph 0065, (2021/06/04)
The present invention relates to a method for synthesis of TKX-50 using an insensitive intermediate and, more specifically, to a method for producing TKX-50, the method comprising the steps of: preparing DCG as a starting material; forming a THP-DAG intermediate from the DCG; and synthesizing TKX-50 through the THP-DAG intermediate.
Synthesis method of 2-pyrazine carboxylic ester compound
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Paragraph 0038; 0045-0047, (2021/04/14)
The invention provides a synthetic method of a 2-pyrazine carboxylic ester compound. The synthesis method comprises the following steps: S1, carrying out addition reaction on a compound 1 and glyoxal dioxime under the action of a Lewis acid catalyst to obtain an intermediate 1; and step S2, carrying out first dehydration reaction on the intermediate 1 to obtain the 2-pyrazine carboxylic ester compound, wherein the structural general formulas of the compound 1, the intermediate 1 and the 2-pyrazine carboxylic ester compound are sequentially shown in the specification, R1 being a C1-C15 substituted or unsubstituted alkyl group, and R2 being a C1-C10 alkyl group. The preparation cost (or commercially available price) of the initial raw material compound 1 adopted by the invention is generally far lower than that of a trifluoropyruvate methyl ester compound. Compared with the traditional preparation method of 3-trifluoromethyl-2-methyl pyrazinecarboxylate, the method has the advantages of mild reaction conditions, simple operation and wide raw material sources, avoids the use of an expensive coupling catalyst, and greatly reduces the cost.
Bis(Substituted Phenylamino)Glyoxime derivatives: Synthesis, characterization, and antimicrobial evaluation
Bayrak, Nilüfer,Matarac?-Kara, Emel,Ozbek-Celik, Berna,Tuyun, Ama? Fatih,Y?ld?r?m, Hatice,Y?ld?z, Mahmut
, (2021/06/16)
In present work, a set of bis(substituted phenylamino) glyoxime derivatives are presented by the dropwise addition of corresponding primary aryl amines to the dichloroglyoxime (1). Reactions of corresponding primary aryl amines containing various substituents in different positions with dichloroglyoxime (1) gave thirteen compounds. The structural characterization of a set of bis(substituted phenylamino) glyoxime derivatives have been performed on the basis of FTIR, mass, proton, and carbon NMR methods. The crystal structure of compound 3a has been determined by X-ray diffraction on a single crystal. The NMR spectrum and X-ray data of 3a show that two hydroxyl groups of dioxime situated at anti position. Furthermore, all of the synthesized compounds (3a-m) were tested for in vitro both antimicrobial activity. The minimal inhibitory concentrations (MICs) against 7 bacteria and 3 yeasts were also determined. Among them, compound 3f was the most potent compound against S. aureus with the value of MIC = 9.76 μg/mL for the antibacterial activity, in addition to this, compound 3i has a good potency against S. aureus and C. tropicalis (MIC = 78.12 μg/mL) for both antibacterial and antifungal activities, respectively.
Synthesis and Synthetic Application of Chloro- And Bromofuroxans
Ando, Akihiro,Hasebe, Hayu,Hayashi, Masahiko,Kim, Hojin,Matsubara, Ryosuke,Tsuneda, Takao
, p. 5959 - 5972 (2020/05/26)
Furoxans are potentially useful heteroaromatic units in pharmaceuticals and agrichemicals. However, the applications for furoxan-based compounds have been hampered due to the underdevelopment of their synthetic methods. Herein, we report a new synthetic approach for the synthesis of chloro- and bromofuroxans. The starting materials were dichloro- and dibromofuroxans, and the substituents were directly introduced to the furoxan ring in a modular fashion. The synthesized monohalofuroxans served as substrates for the installation of a second substituent to prepare further functionalized furoxans.
SYNTHESIS OF TKX-50 USING INSENSITIVE INTERMEDIATE
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Paragraph 0059; 0060, (2020/05/01)
The present invention relates to a method for synthesizing TKX-50 using an insensitive intermediate. More specifically, the present invention relates to a method for manufacturing TKX-50 comprising the following steps: preparing DCG as a starting material; forming a THP-DAG intermediate from the DCG; and synthesizing TKX-50 through the THP-DAG intermediate. The present invention allows an operator to synthesize TKX-50 more safely.(AA) Glyoxal(BB) GlyoximeCOPYRIGHT KIPO 2020
SYNTHESIS OF TKX-50 USING INSENSITIVE INTERMEDIATE
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Paragraph 0024; 0059-0060, (2020/06/06)
TKX-50 Is a method for synthesizing, using an obtuse intermediate, in which DCG is prepared from the starting material; and DCG is formed from THP-DAG, and; is synthesized through the THP-DAG intermediate. TKX-50. The method of; comprising the steps, TKX-50 and. (by machine translation)
FUNCTIONALITY PROTECTED DIAZIDOGLYOXIME AND SYNTHESIS METHOD OF THE SAME
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Paragraph 0087-0090, (2020/06/09)
Is a,sectional view of a diazidoglycol protected with a functional group according to an embodiment of the present invention 1, which is represented by the following Formula : [Formula 1] (Wherein, R denotes tetrahydropyranyl (Tetrahydropyranyl; THP), methyl (Methyl; Me), methoxymethyl (Methoxymethyl; MOM),methoxymethyl (Methoxythiomethyl; MTM),methoxymethyl (Benzyloxymethyl; BOM), 2- methoxymethyl-(2-Methoxymethyl; MEM), 2-(-methoxymethyl)-methoxybenzyl ((2-(Trimethylsilyl)ethoxymethyl); SEM), trimethylsilyl-(Tetrahydrofuranyl; THF), t-methoxyethyl-(t-Butyl),methoxyethyl-(Allyl),trimethoxyacetate (Benzyl), p- dimethoxymethyl (p-Methoxybenzyl), 3,4-methylsilyl (3,4-Dimethoxybenzyl), o-trimethoxyethyl] (o-Nitrobenzyl), p-trimethoxyethyl -t- triethylsilyl (p-Nitrobenzyl),trimethoxyethyl] (Chloroacetate),butyl (Triphenylmethyl), (Triphenylmethoxyacetate),methylsilyl-(Benzoate) hexyl p- (Di-t-butylmethylsilyl; DTBMS), (Trimethylsilyl; TMS),(Acetate; Ac), methoxybenzyl (Triethylsilyl; TES),(Methoxyacetate), trimethoxyethyl] (Pivaloate), (Triisopropylsilyl; TIPS), t-trimethoxyethyl (p-Toluenesulfonate; Ts). (t-Butyldimethylsilyl; TBDMS), t-trimethoxyethyl]-butyl-(t-Butyldiphenylsilyl; TBDPS),).methylsilyl-triethylsilyl-trimethoxyethyl]-benzenesulfonate (Diphenylmethylsilyl; DPMS). (by machine translation)
