📜3-甲基-3-戊烯-2-酮置于palladium On Activated Charcoal,氢气体系中,85.0 °C,1.0 Mpa 条件下,反应 3.5H,以1.2 Kg的收率获得产物3-甲基-2-戊酮 参考文献:5-Sec-Butyl-2-(2,4-Dimethyl-Cyclohex-3-Enyl)-5-Methyl-[1,3]Dioxane And Process For Making The Same 标题:5-Sec-Butyl-2-(2,4-Dimethyl-Cyclohex-3-Enyl)-5-Methyl-[1,3]Dioxane And Process For Making The Same 摘要:本发明涉及5-Sec-丁基-2-(2,4-二甲基环己-3-烯基)-5-甲基-[1,3]二噁烷及其制备的新方法.
专利号:US-9518047-B2 优先权日:2013-10-17 标题 :Process for the industrial synthesis of lurasidone 发明人:ANGELINI TOMMASO; BETTONI PIERGIORGIO; ROLETTO JACOPO; PAISSONI PAOLO 权利人:PROCOS SPA 摘要:Disclosed is a process for the industrial synthesis of Lurasidone from (1R,2R)-cyclohexane-1,2-diyldimethanol (1), 3-(piperazin-1-yl)benzo[d]isothiazole (3) and (3aR,4R,7R,7aS)-3a,4,7,7a-tetrahydro-4,7-methanoisobenzofuran-1,3-dione (6).). Said process is optimised to obtain Lurasidone with high yields and high purities by preparing highly pure synthesis intermediates, using critical raw materials and reagents in amounts close to the stoichiometric amounts, increasing productivity and reducing the costs and environmental impact of the process.
专利号:US-8791287-B2 优先权日:2010-07-02 标 题:Process for the synthesis of tapentadol and intermediates thereof 发明人:MOTTA GIUSEPPE; VERGANI DOMENICO; BERTOLINI GIORGIO; LANDONI NICOLA 权利人:MOTTA GIUSEPPE; VERGANI DOMENICO; BERTOLINI GIORGIO; LANDONI NICOLA; EUTICALS SPA 摘要:The object of the present invention is a new process for the synthesis of tapentadol, both as free base and in hydrochloride form, which comprises the step of alkylation of the ketone (VII) to yield the compound (VIII), as reported in Diagram 1, with high stereoselectivity due to the presence of the benzyl group as substituent of the amino group. It was surprisingly found that this substitution shifts the keto-enol equilibrium towards the desired enantiomer and amplifies the capacity of the stereocenter present in the compound (VII) to orient the nucleophilic addition of the organometallic compound at the carbonyl towards the desired stereoisomer. This substitution thus allows obtaining a considerable increase of the yields in this step, and consequently allows significantly increasing the overall yield of the entire tapentadol synthesis process. n A further object of the present invention is constituted by the tapentadol free base in solid form, obtainable by means of the process of the invention. n Still another object of the invention is represented by the crystalline forms I and II of the tapentadol free base. n A further object of the present invention is the mixture of the crystalline forms I and II of the tapentadol free base.
专利号:US-7294743-B2 优先权日:2003-10-23 标题:Method for synthesis of acrylamide derivatives 发明人:ALGOTSSON MATTIAS; BUSSON PHILIPPE; THEVENIN NICOLAS 权利人:GE HEALTHCARE BIO SCIENCES AB 摘要:The present invention relates to a method for synthesis of an acrylamide derivative, starting with dissolving a salt of a nucleophilic amine in water to form an aqueous solution and desalting said solution with a base, comprising the following steps:n a) addition of dissolved activated acrylic acid derivative to said solution; b) acidification of aqueous phase; and c) extraction of said aqueous phase.
专利号:US-2010087525-A1 优先权日:2008-06-23 标 题:Stereoselective enzymatic synthesis of (s) or (r)-iso-butyl-glutaric ester 发明人:HEDVATI LILACH; STERIMBAUM GRETA; RAIZI YURIY; AMINOV RAHAMIN 权利人:HEDVATI LILACH; STERIMBAUM GRETA; RAIZI YURIY; AMINOV RAHAMIN 摘要:The present invention relates to a stereoselective enzymatic synthesis of (S) or (R)-iso-butyl-glutaric ester, an intermediate of S-Pregabalin.
专利号:US-9126896-B2 优先权日:2012-06-01 标题:Synthesis of diamido gellants by using Dane salts of amino acids 发明人:BINDL MARTIN; HERRMANN ROLAND; KNAUP GUNTER 权利人:EVONIK INDUSTRIES AG 摘要:The invention relates to a method for the synthesis of a compound according to formula I comprising the following steps: a) reacting a Dane salt according to formula II and a Dane salt according to formula III with a coupling reagent; b) adding a diamine according to formula IV to the reaction mixture; and c) adding an acid to the reaction mixture to adjust the pH value of the reaction to <7; wherein L represents a C 2 -C 20 alkyl group, a C 6 -C 20 aryl group, or a C 7 -C 20 alkylaryl group; R 1 and R 2 can be identical or different and represent a hydrogen atom, a C 1 -C 4 alkyl group, a C 1 -C 4 hydroxyalkyl group, a C 1 -C 4 thioether group, a C 6 -C 20 aryl group, a C 7 -C 20 alkylaryl group, a C 7 -C 20 alkylhydroxyaryl group, a C 4 -C 20 alkylheteroaryl group with 1 to 4 heteroatoms; or a C 1 -C 4 alkylcarboxylic moiety, which may be an acid, an amide, or which may be esterified with a C 1 -C 6 alkyl group or a C 7 -C 20 alkylaryl group; R 3 represents a C 1 -C 4 alkyl group; R 4 represents a hydrogen atom, or a C 1 -C 4 alkyl group; R 5 represents a C 1 -C 4 alkyl group; and X represents an alkali metal.
专利号:US-11459303-B2 优先权日:2019-06-21 标题 :Process for the synthesis of lofexidine 发明人:DONNOLA MONICA; BAROZZA ALESSANDRO; ROLETTO JACOPO; PAISSONI PAOLO 权利人:PROCOS SPA 摘要:Disclosed is a process for the synthesis of lofexidine of formula (I) and the hydrochloride salt thereof (II), from ethyl 2-(2,6-dichlorophenoxy)propionate (III) and ethylenediamine in the presence of tetravalent titanium alkoxides, preferably titanium isopropoxide, in an apolar solvent such as toluene. A further object of the present invention is a process for the preparation of the intermediate ethyl 2-(2,6-dichlorophenoxy)propionate (III) from 2,6-dichlorophenol and ethyl 2-chloropropionate in the presence of a polar aprotic solvent and an alkali or alkaline earth carbonate salt, preferably potassium carbonate. Both processes are more cost-effective and more easily industrially scalable than the known procedures, thus enabling the active ingredient to be obtained with high yields at a limited cost.
摘要:Smith, L. H. S.; Coote, S. C.; Procter, D. J., Science of Synthesis Knowledge Updates, (2010) 3, 479. 摘要:Faber, K.; Hall, M., Science of Synthesis: Biocatalysis in Organic Synthesis, (2015) 2, 217. 参考文献:10.1023/b:jcam.0000005764.26206.74 摘要:Ren B. New atom-type-based AI topological indices: Application to QSPR studies of aldehydes and ketones. Journal of Computer-Aided Molecular Design. 2003 Sep;17(9):607–19. doi: 10.1023/b:jcam.0000005764.26206.74.