专利号:US-7767826-B2 优先权日:2007-10-05 标题 :Process for the synthesis of L-(+)-ergothioneine 发明人:TRAMPOTA MIROSLAV 权利人:PHARMATECH INTERNATIONAL INC 摘要:This invention relates to a novel process for the preparation of optically pure L-(+)-ergothioneine. The process for the chemical synthesis of L-ergothioneine comprises steps which consist of reacting L-histidine alkyl ester with an acid halide, chloroformate or pyrocarbonate in the presence of a base, hydrolysis of the alkyl-(S,Z)-2,4,5-triamidopent-4-enoate to obtain a (S)-alkyl 2,5-diamido-4-oxopentanoate, acid catalyzed hydrolysis of the (S)-alkyl 2,5-diamido-4-oxopentanoate followed by reaction with a metal thiocyanate to obtain the thiohistidine, protection of the sulfur of thiohistidine as the tert-butyl thioether, dialkylation of the primary amine to obtain a tertiary amine, quaternization of the tertiary amine, and removal of the protecting group to obtain the desired (S)-3-(2-mercapto-1H-imidazol-5-yl)-2-(trialkylammonio)propanoate (I). This process affords a better yield and is capable of practical application at large scale.
专利号:US-11945764-B2 优先权日:2021-06-09 标 题:Efficient synthesis of diglycolamide molecules 发明人:JANSONE-POPOVA SANTA; POPOVS ILJA 权利人:UT BATTELLE LLC 摘要:A method for producing a diglycolamide molecule having the formula: n nwherein R 1 and R 2 are independently selected from alkyl groups (R) and acyl groups (C(O)R) in which the alkyl groups (R) contain 1-30 carbon atoms and optionally contain an ether or thioether linkage between carbon atoms, and R 5 and R 6 are independently selected from hydrogen atom and alkyl groups containing 1-3 carbon atoms; and one or both pairs of R 1 and R 2 are optionally interconnected to form a ring; the method comprising: combining a diglycolic acid molecule (A) and a secondary amine (B) to form a salt intermediate (C), and heating the salt intermediate (C) to a temperature of 100° C. to 300° C. to form the diglycolamide of Formula (1) in a dehydration process, wherein the method is shown schematically as follows:
专利号:US-9790377-B2 优先权日:2011-09-21 标题:Synthesis of functional fluorinated polyhedral oligomeric silsesquioxane (“F-POSSâ€?) 发明人:HADDAD TIMOTHY S; MABRY JOSEPH M; RAMIREZ SEAN 权利人:US AIR FORCE 摘要:A method of manufacturing a fluorinated polyhedral oligomeric silsesquioxane. The method for manufacture includes opening a single edge of a closed-cage F-POSS and bridging the opened, single edge with a sulfate group. The sulfate group is converted to a disilanol, which is then reacted with a functional dichlorosilane having an organic functional group comprising at least three carbon atoms.
专利号:US-2009093642-A1 优先权日:2007-10-05 标 题 :Process for the synthesis of l-(+)-ergothioneine
专利号:WO-2009045413-A1 优先权日:2007-10-05 标 题 :Process for the synthesis of l-(+)-ergothioneine
专利号:US-2023002311-A1 优先权日:2021-06-09 标 题 :Efficient synthesis of diglycolamide molecules
[参考文献]: Ervin Sz Kováts, Et Al. Wrong Gas/liquid Partition Data By Gas Chromatography. J Chromatogr A. 2006 Apr 28;1113(1-2):206-19.
合成参考文献
摘要:Eilbracht, P., Science of Synthesis, (2009) 48, 394. 摘要:Kantchev, E. A. B.; Organ, M. G., Science of Synthesis, (2009) 48, 38. 摘要:Kantchev, E. A. B.; Organ, M. G., Science of Synthesis, (2009) 48, 30. 摘要:Song, Z.; Takahashi, T., Science of Synthesis Knowledge Updates, (2013) 1, 81. 摘要:Oishi, M.; Takikawa, H., Science of Synthesis Knowledge Updates, (2010) 4, 104.