Combustion synthesis of zero-, one-, two- and three-dimensional nanostructures: Current trends and future perspectives

Nersisyan, Hayk H.,Lee, Jong Hyeon,Ding, Jin-Rui,Kim, Kyo-Seon,Manukyan, Khachatur V.,Mukasyan, Alexander S. Elsevier 2017 Progress in energy and combustion science Vol.63 No.-

<P><B>Abstract</B></P> <P>The combustion phenomenon is characterized by rapid self-sustaining reactions, which can occur in the solid, liquid, or gas phase. Specific types of these reactions are used to produce valuable materials by different combustion synthesis (CS) routes. In this article, all three CS approaches, i.e. solid-phase, solution, and gas-phase flame, are reviewed to demonstrate their attractiveness for fabrication of zero-, one-, two-, and three-dimensional nanostructures of a large variety of inorganic compounds. The review involves five sections. First, a brief classification of combustion synthesis methods is given along with the scope of the article. Second, the state of art in the field of solid-phase combustion synthesis is described. Special attention is paid to the relationships between combustion parameters and structure/properties of the produced nanomaterials. The third and fourth sections describe details for controlling material structures through solution combustion synthesis and gas-phase flame synthesis, respectively. A variety of properties (e.g., thermal, electronic, electrochemical, and catalytic) associated with different types of CS nanoscale materials are discussed. The conclusion focuses on the most promising directions for future research in the field of advanced nanomaterial combustion synthesis.</P>

A novel synthetic method of peptide nucleic acid (PNA) oligomers using Boc/Cbz-protected PNA trimer blocks in the solution phase

Periyalagan Alagarsamy,Hong In Seok 대한화학회 2022 Bulletin of the Korean Chemical Society Vol.43 No.5

In order to use peptide nucleic acid (PNA) oligomers for therapeutic purposes, a high purity level is essential and, in particular, large-scale production should be easy. However, in the traditional solid-phase synthesis method, the generation of n 1 or n 2 deleted oligomers cannot be completely excluded, and purification of crude oligomers is difficult because the target and impurities overlap. Also, for these reasons, scale-up is also limited. Here, we report the efficient synthesis of PNA oligomers in the solid phase using fully protected PNA trimers instead of monomers. Fully protected PNA trimer blocks were successfully synthesized via two different routes in the solution phase. When PNA oligomers were synthesized in the solid phase using trimer blocks as monomers, a higher purity level of PNA could be synthesized compared to when oligomers were synthesized using monomers. When using this method, n 1 or n 2 truncated products cannot be systematically produced. Furthermore, the trimer blocks coupling method is successful even for sequences containing purinerich and/or gamma PNAs, which are difficult to synthesize via the conventional solid-phase peptide synthesis approach. Finally, two hexameric and one dodecameric PNA oligomers were completely synthesized in the solution phase, with the former showing more than 90% crude purity and the latter showing 70%. We propose that this method may be able to solve several problems related to solid-phase synthesis at once.

Combinatorial Solid Phase Peptide Synthesis and Bioassays

Shin, Dong-Sik,Kim, Do-Hyun,Chung, Woo-Jae,Lee, Yoon-Sik Korean Society for Biochemistry and Molecular Biol 2005 Journal of biochemistry and molecular biology Vol.38 No.5

Solid phase peptide synthesis method, which was introduced by Merrifield in 1963, has spawned the concept of combinatorial chemistry. In this review, we summarize the present technologies of solid phase peptide synthesis (SPPS) that are related to combinatorial chemistry. The conventional methods of peptide library synthesis on polymer support are parallel synthesis, split and mix synthesis and reagent mixture synthesis. Combining surface chemistry with the recent technology of microelectronic semiconductor fabrication system, the peptide microarray synthesis methods on a planar solid support are developed, which leads to spatially addressable peptide library. There are two kinds of peptide microarray synthesis methodologies: pre-synthesized peptide immobilization onto a glass or membrane substrate and in situ peptide synthesis by a photolithography or the SPOT method. This review also discusses the application of peptide libraries for high-throughput bioassays, for example, peptide ligand screening for antibody or cell signaling, enzyme substrate and inhibitor screening as well as other applications.

Current Parallel Solid-Phase Synthesis of Drug-like Oxadiazole and Thiadiazole Derivatives for Combinatorial Chemistry

Abdildinova, Aizhan,Gong, Young-Dae American Chemical Society 2018 ACS Combinatorial Science Vol.20 No.6

<P>Solid-phase organic synthesis is a powerful tool in the synthesis of small organic molecules and building of libraries of compounds for drug discovery. Heterocyclic compounds are important components of the drug discovery field as well and serve as a core for hundreds of marketed drugs. In particular, oxadiazole and thiadiazole cores are compounds of great interest due to their comprehensive biological activities and structural features. Therefore, a plethora of oxadiazole and thiadiazole synthesis methodologies have been reported to date, including solution and solid-phase synthesis methodologies. In this review, we concentrate on and summarize solid-phase synthetic approaches of the oxadiazole and thiadiazole derivatives.</P> [FIG OMISSION]</BR>

A novel solid-phase synthetic method for production of <i>N</i>-alkyl-4-alkylamino-1-aryl-1<i>H</i>-pyrazolo[3,4-<i>d</i>]pyrimidine-6-carboxamide library

Heo, Yun-Jeong,Jeon, Moon-Kook Elsevier 2017 Tetrahedron Vol.73 No.40

<P><B>Abstract</B></P> <P>This work describes a solid-phase synthetic method for building a compound library of <I>N</I>-alkyl-4-alkylamino-1-aryl-1<I>H</I>-pyrazolo[3,4-<I>d</I>]pyrimidine-6-carboxamide derivatives, that are based on the biologically active 1-aryl-1<I>H</I>-pyrazolo[3,4-<I>d</I>]pyrimidine scaffold. In the first step of this synthetic sequence, condensation reactions of ethyl 5-amino-1-aryl-1<I>H</I>-pyrazole-4-carboxylates with methyl cyanoformate resulted in the formation of esters that underwent hydrolysis to give 1-aryl-4,5-dihydro-1<I>H</I>-pyrazolo[3,4-<I>d</I>]pyrimidin-4-one-6-carboxylic acids. The coupling reaction of these carboxylic acids with primary alkylamine-loaded acid-sensitive methoxybenzaldehyde (AMEBA) resins was followed by amination reactions mediated by benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (BOP). Subsequent cleavage from the solid support resulted in the formation of the target <I>N</I>-alkyl-4-alkylamino-1-aryl-1<I>H</I>-pyrazolo[3,4-<I>d</I>]pyrimidine-6-carboxamide derivatives. The reaction conditions for solid-phase transformations were optimized using a solution-phase model study with 2,4-dimethoxybenzyl-protected isobutylamine as a reactant in place of the AMEBA resin-loaded isobutylamine. The progress of the solid-phase reactions was monitored by on-bead ATR-FTIR spectroscopy. Diversification experiments were performed by using 1-aryl-4,5-dihydro-1<I>H</I>-pyrazolo[3,4-<I>d</I>]pyrimidin-4-one-6-carboxylic acids and a variety of primary and secondary amine building blocks to build the target compound library.</P> <P><B>Graphical abstract</B></P> <P>[DISPLAY OMISSION]</P>

Fabrication of Monodisperse and Mechanically Controllable PEG -Acrylated Microgel beads for Solid-Phase Peptide Synthesis

김성수,이상명,신동식 한국공업화학회 2020 한국공업화학회 연구논문 초록집 Vol.2020 No.-

Droplet microfluidics combined with addition polymerization of acrylate monomers is an attractive technology to control micro-scaled skeletal architecture.[1] Recently, there are widespread reports of PEG hydrogels that is suitable for water compatiblility and anti-fouling.[2] In this study, microgel beads prepared from poly(ethylene glycol) methyl ether acrylate (PEGA) and poly(ethylene glycol) diacrylate (PEGDA) are characterized for mechanical properties. This mechanically controllable PEG hydrogel bead was successfully performed for solid -phase peptide synthesis. The loading level and purity of tripeptides were evaluated to evaluate coupling efficiency. The synthesis and application of SPPS is described in order to offer the suitable technology of pharmaceutical ingredient production.

Synthesis of Silicon Tracelsss Linker for Solid-Phase Reaction

Mun Han-Seo,Seong Jin-Hyun The Pharmaceutical Society of Korea 2004 Archives of Pharmacal Research Vol.27 No.4

The silicon linker is the foremost traceless linker used in solid-phase reactions. Hydrogen fluo-ride (HF) or trifluoroacetic aicd (TFA) can remove the silicon linker with the silicon atom being replaced by a hydrogen atom. In this experiment, the linkers 1c and 2d, which are the most useful in solid-phase reactions, were synthesized, Linker 1c is composed of seven linearly linked carbons and linker 2d includes an oxygen atom in the linear carbon chain to increase the solvation capacity. The carboxylic acid component of linker 1c and 2d forms an amide or ester bond with resin. The synthesized linkers 1c and 2d could be utilized in constructing a chemical compound library that includes indole, benzodiazepine and phenothiazine (aromatic ring compounds).

The Solid-Phase Synthesis of Amino Acid-Derived Diacetylene Lipids

Kim Jong-Man,Park Bum Jun,Chang Eun-Ju,Yi Sung Chul,Suh Dong Hack,Ahn Dong June The Polymer Society of Korea 2005 Macromolecular Research Vol.13 No.3

We prepared amino acid-derived diacetylene monomers using solid-phase organic synthesis. The solid-phase synthetic method allowed for the rapid and efficient preparation of functional diacetylenes. Amino acids having hydrophobic sidechains such as alanine, leucine, and phenylalanine, as well as hydrophilic sidechains such as aspartic acid and lysine, were successfully coupled to the diacetylene lipid. The diacetylene monomers prepared in this way were subjected to routine procedures for the generation of polydiacetylene vesicles. Depending on the nature of the side-chains, pink to blue colored polydiacetylenes were generated.

Batimastat의 고체상 합성법에 관한 연구

김지연,임세진 동덕여자대학교 종합약학연구소 2001 동덕약학연구지 Vol.5 No.-

The solid-phase approach to the facile synthesis of batimastat is described. Acid compound (5), prepared by solution-phase synthesis is loaded to a acid labile resin bearing a hydroxylamine linker and is subjected to a stereoselective Michael addition and subsequent acidic cleavage, affording batimastat in good yield and in short period of time.

Synthesis of Silicon Traceless Linker for Solid-Phase Reaction

Han-Seo Mun,정진현 대한약학회 2004 Archives of Pharmacal Research Vol.27 No.4

The silicon linker is the foremost traceless linker used in solid-phase reactions. Hydrogen fluoride (HF) or trifluoroacetic aicd (TFA) can remove the silicon linker with the silicon atom being replaced by a hydrogen atom. In this experiment, the linkers 1c and 2d, which are the most useful in solid-phase reactions, were synthesized. Linker 1c is composed of seven linearly linked carbons and linker 2d includes an oxygen atom in the linear carbon chain to increase the solvation capacity. The carboxylic acid component of linker 1c and 2d forms an amide or ester bond with resin. The synthesized linkers 1c and 2d could be utilized in constructing a chemical compound library that includes indole, benzodiazepine and phenothiazine (aromatic ring compounds).