乙烯酮置于硫化氢,三乙胺体系中,用 正丁醇 作为反应溶剂,以65%的收率获得产物硫代乙酸 参考文献:[de] Verfahren Zur Herstellung Von Thioessigsäure Und Ihren Salzen Method For The Production Of A Thioacetic Acid And Salts Thereof[fr] Procede Pour Produire Un Acide Thioacetique Et Ses Sels 标题:[de] Verfahren Zur Herstellung Von Thioessigsäure Und Ihren Salzen Method For The Production Of A Thioacetic Acid And Salts Thereof[fr] Procede Pour Produire Un Acide Thioacetique Et Ses Sels 摘要:该发明涉及一种制备硫代乙酸及其盐的方法,其中mn+表示铵或碱金属,碱土金属,铝或钛阳离子,通过在氮碱存在下将烯与硫化氢反应或将烯与水溶性碱金属氢硫化物溶液反应.所形成的硫代乙酸随后可以通过与氨或碱金属,碱土金属,铝或钛碱反应转化为相应的盐.优选将硫代乙酸的反应和盐的形成作为"一锅法"进行.
专利号:US-6013829-A 优先权日:1996-02-05 标 题 :Process for the asymmetric synthesis of S-acyl derivatives of 2-mercaptomethyl -3- phenyl propanoic acid, application to the synthesis of N-(mercaptoacyl) amino acid derivatives 发明人:DANVY DENIS; MONTEIL THIERRY; DUHAMEL PIERRE; DUHAMEL LUCETTE; LECOMTE JEANNE-MARIE; SCHWARTZ JEAN-CHARLES; NOEL-LEFEBVRE NADINE; GROS CLAUDE; PLAQUEVENT JEAN-CHRISTOPHE 权利人:BIOPROJET SOC CIV 摘要:PCT No. PCT/FR97/00218 Sec. 371 Date Nov. 26, 1997 Sec. 102(e) Date Nov. 26, 1997 PCT Filed Feb. 4, 1997 PCT Pub. No. WO97/29086 PCT Pub. Date Aug. 14, 1997Process for the asymmetric synthesis of S-acyl derivatives of 2-mercaptomethyl-3-phenylpropanoic acid of formula (I): characterized in that it comprises the steps consisting in: a) preparing the diol (VI) by reduction of a malonic ester (V) in the presence of a hydride; b) preparing the monoacetates (VII R) or (VII S) respectively; c) subjecting these monoacetates to an oxidation in order to form the acids (IX S) or (IX R); d) saponifying the compounds (IX S) or (IX R) in order to form the hydroxy acids (X S) or (X R); e) thioacylating the hydroxy acids (X S) or (X R) with a mercapto acid R1SH (XI), according to a Mitsunobu-type reaction, in order to lead to the desired acids (I R) (I S) respectively and application to the synthesis of N-(mercaptoacyl)amino acid derivatives (II).
专利号:WO-2020215726-A1 优先权日:2019-04-26 标题:Recycling process of waste generated in synthesis of thioacetic acid 发明人:ZHANG SHIJIN; ZHANG XIANGZHOU; LIU DUNSHENG; MA ZHAOFENG 权利人:TENGZHOU TIANSHUI BIO TECH CO LTD 摘要:A recycling process of waste generated in synthesis of thioacetic acid, comprising: in a thioacetic acid synthesis process, pretreating a thioacetic acid synthesis reaction solution, transferring the reaction solution to a filter device, separating a solid phase from a liquid phase in the reaction solution, and separating waste from the reaction solution in advance; and treating the separated solid phase: washing the solid phase, and performing separation after the washing; feeding the washed solid phase into a drier for drying, separating the dried solid, and condensing the liquid phase; adding the dried solid into a dissolving kettle, adding water into the kettle, stirring and heating to micro-boiling and reflux, so that the dried solid is fully dissolved; then adding a potassium hydroxide solution into the solution for neutralization, during which boiling should be prevented and which lasts for not shorter than 5 min; filtering a neutralization solution, and separating solid precipitate therefrom; neutralizing a filtrate obtained after the filtration to perform evaporative concentration, and primarily separating water from monopotassium phosphate; performing a further separation operation on a monopotassium phosphate concentrated solution, the solid obtained after the separation being a monopotassium phosphate product; and repeating the previous step for re-concentration.
专利号:US-7230101-B1 优先权日:2002-08-28 标 题:Synthesis of methotrexate-containing heterodimeric molecules 发明人:MURTHI KRISHNA K; SMITH CHASE C 权利人:GPC BIOTECH INC 摘要:The present invention relates to novel compositions of methotrexate-containing heterodimeric probe molecules, also known as chemical inducers of dimerization (CID), useful in three-hybrid assays. The invention further relates to synthesis of said compositions and their intermediates. Another aspect of the invention is a method for using the heterodimeric probe molecules described herein in drug screens to identify potential protein targets to a given ligand, optimize protein-ligand interactions, or identify potential ligands for a given protein target. In certain embodiments, the invention contemplates the synthesis of the following methotrexate-containing heterodimeric probe:
专利号:US-2004058888-A1 优先权日:2000-01-13 标题:Methods for synthesis of alpha-d-gal (1~>3) gal-containing oligosaccharides 发明人:BORNAGHI LAURENT; DEKANY GYULA; DRINNAN NICHOLAS BARRY; PAPAGEORGIOU JOHN; WEST MICHAEL LEO 摘要:This invention relates to reagents and methods for synthesis of biologically active di- and tri-saccharides comprising α-D-Gal(1→3)-D-Gal. In particular the invention provides novel reagents, intermediates and processes for the solution or solid phase synthesis of α-D-galactopyranosyl-(1→3)-D-galactose, and derivatives thereof. In one preferred embodiments the invention provides a protected monosaccharide building block of general formula (II): in which R 3 is methoxy or methyl; R 1 is H, benzoyl, pivaloyl, 4-chlorobenzoyl, acetyl, chloroacetyl, levulinoyl, 4-methylbenzoyl, benzyl, 3,4-methylenedioxybenzyl, 4-methoxybenzyl, 4-chlorobenzyl, 4-acetamidobenzyl, or 4-azidobenzyl; and R 2 is H, Fmoc, benzoyl, pivaloyl, 4-chlorobenzoyl, acetyl, chloroacetyl, levulinoyl, 4-methylbenzoyl, benzyl, 3,4-methylenedioxybenzyl, 4-methoxybenzyl, 4 -chlorobenzyl, 4-acetamidobenzyl, or 4-azidobenzyl.
专利号:US-2013267680-A1 优先权日:2010-09-15 标题:Total chemical synthesis of ubiquitin, ubiquitin mutants and derivatives thereof 发明人:OVAA HUIB; EL OUALID FARID; MERKX REMCO NICOLAAS SEBASTIAAN MICHEL 权利人:OVAA HUIB; EL OUALID FARID; MERKX REMCO NICOLAAS SEBASTIAAN MICHEL; STICHTING HET NL KANKERINST 摘要:The present invention relates to the field of total chemical synthesis of ubiquitin and related peptides. More in particular, a method is provided of solid phase synthesis of ubiquitin, ubiquitin mutants and derivatives thereof. It was the object of the present invention to provide an approach for the total chemical synthesis of ubuiqitin, which allows for the chemical synthesis of virtually any Ub mutant and giving high overall efficiency and purity. The present inventors have surprisingly found that this object can be realized with a method relying on incorporation of special amino acid building blocks. This approach was found to allow for exceptionally high yields of up to 14% and to provide an synthetic entry into virtually any ubiquitin derivative.
专利号:US-11046978-B2 优先权日:2016-03-16 标 题:Synthesis of isoprenoids and derivatives 发明人:GONZALEZ RAMON; CLOMBURG JAMES M; CHEONG SEOKJUNG 权利人:UNIV RICE WILLIAM M 摘要:This disclosure generally relates to the use of enzyme combinations or recombinant microbes comprising same to make isoprenoid precursors, isoprenoids and derivatives thereof including prenylated aromatic compounds. Novel metabolic pathways exploiting Claisen, aldol, and acyioin condensations are used instead of the natural mevalonate (MVA) pathway or 1-deoxy-d-xylulose 5-phosphate (DXP) pathways for generating isoprenoid precursors such as isopentenyl pyrophosphate (IPP), dimethylallyl pyrophosphate (DMAPP), and geranyl pyrophosphate (GPP). These pathways have the potential for better carbon and or energy efficiency than native pathways. Both decarboxylative and non-carboxylative condensations are utilized, enabling product synthesis from a number of different starting compounds. These condensation reactions serve as a platform for the synthesis of isoprenoid precursors when utilized in combination with a variety of metabolic pathways and enzymes for carbon rearrangement and the addition/removal of functional groups. Isoprenoid alcohols are key intermediary products for the production of isoprenoid precursors in these novel synthetic metabolic pathways.
摘要:Yoshikai, N.; Rayner, C. M.; Graham, M. A., Science of Synthesis Knowledge Updates, (2020) 2, 67. 摘要:Koutentis, P. A.; Ioannidou, H. A., Science of Synthesis Knowledge Updates, (2010) 1, 273. 摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2018) 2, 169. 摘要:Wang, M.; Jiang, X., Science of Synthesis Knowledge Updates, (2021) 2, 224. 摘要:Croft, R. A.; Bull, J. A., Science of Synthesis Knowledge Updates, (2018) 4, 417.