专利号:WO-2009018504-A1 优先权日:2007-08-01 标题 :Process for the synthesis of diaminopyridine and related compounds 发明人:RITTER JOACHIM C 权利人:DU PONT; RITTER JOACHIM C 摘要:A process is provided for the synthesis of a diaminopyridine, such as 2,6-diaminopyridine and related compounds, which are used industrially as compounds and as components in the synthesis of a variety of useful materials. The synthesis proceeds by means of a chlorine-ammonia displacement in the presence of a copper source.
专利号:US-8222458-B2 优先权日:2008-06-13 标题 :Process or synthesis of (3S)- and (3R)-3-hydroxy-beta-ionone, and their transformation to zeaxanthin and beta-cryptoxanthin 发明人:KHACHIK FREDERICK; CHANG AN-NI 权利人:KHACHIK FREDERICK; CHANG AN-NI; UNIV MARYLAND 摘要:Disclosed is a process for the synthesis of (3R)-3-hydroxy-β-ionone and its (3S)-enantiomer in high optical purity from commercially available (rac)-α-ionone. The key intermediate for the synthesis of these hydroxyionones is 3-keto-α-ionone ketal that was prepared from (rac)-α-ionone after protection of this ketone as a 1,3-dioxolane. Reduction of 3-keto-α-ionone ketal followed by deprotection, lead to 3-hydroxy-α-ionone that was transformed into (rac)-3-hydrox-β-ionone by base-catalyzed double bond isomerization in 46% overall yield from (rac)-α-ionone. The racemic mixture of these hydroxyionones was then resolved by enzyme-mediated acylation in 96% ee. (3R)-3-Hydroxy-β-ionone and its (3S)-enantiomer were respectively transformed to (3R)-3-hydroxy-(β-ionylideneethyl)triphenylphosphonium chloride [(3R)-C 15 -Wittig salt] and its (3S)-enantiomer [(3S)-C 15 -Wittig salt] according to known procedures. Double Wittig condensation of these Wittig salts with commercial available 2,5- dimethtylocta-2,4,6-triene-1,8-dial provided all 3 stereoisomers of zeaxanthin. Similarly, (3R)-C 15 -Wittig and its (3S)-enantiomer were each coupled with β-apo-12′-carotenal.
专利号:US-7858828-B2 优先权日:2008-03-26 标 题 :Process for synthesis of (3R,3'R,6'R)-lutein and its stereoisomers 发明人:KHACHIK FREDERICK; CHANG AN-NI 权利人:UNIV MARYLAND 摘要:(3R,3′R,6′R)-Lutein and (3R,3′R)-zeaxanthin are two dietary carotenoids that are present in most fruits and vegetables commonly consumed in the US. These carotenoids accumulate in the human plasma, major organs, and ocular tissues. In the past decade, numerous epidemiological and experimental studies have shown that lutein and zeaxanthin play an important role in the prevention of age-related macular degeneration (AMD) that is the leading cause of blindness in the U.S. and Western World. The invention provides a process for the synthesis of (3R,3′R,6′R)-lutein and its stereoisomers from commercially available (rac)-α-ionone by a C 15 +C 10 +C 15 coupling strategy. In addition, the present invention also provides access to the precursors of optically active carotenoids with 3-hydroxy-ε-end group that are otherwise difficult to synthesize. The process developed for the synthesis of lutein and its stereoisomers is straightforward and has potential for commercialization.
专利号:US-4284582-A 优先权日:1978-04-28 标 题 :Process for the preparation of cyclopropane derivatives, intermediates in the synthesis of pyrethroid insecticides 发明人:KAYE ALBERT E; TUCKER ALAN C 权利人:ICI LTD 摘要:Compounds of formula: wherein both groups X are chlorine, bromine or trifluoromethyl, or one X is chlorine or bromine and the other is trifluoromethyl, and Y is -CN or -COOR in which R is an alkyl group, are obtained by (A) reacting a compound of the formula: wherein X1 is chlorine or bromine, with a compound of the formula: X2C=CH-CH=C(CH3)2 in the presence of metallic copper or at least one copper salt and a base, or (B) reacting a compound of the formula: Y-CH2-CN with a compound of the formula: X2C=CH-CH=C(CH3)2 and chlorine or bromine, in the presence of at least one reducible copper salt and a base, or (C) reacting a compound of formula: X-CH2-CN with a compound of the formula: wherein X1 is chlorine or bromine, in the presence of at least one copper salt. The compounds are intermediates in the synthesis of pyrethroid insecticides.
专利号:US-7691968-B2 优先权日:2002-05-03 标题:Process for the synthesis of peptides amides by side-chain attachment to a solid phase 发明人:EVANS DAVID JOHN; SIMPKIN DEAN STEVEN ANTHONY; WELLINGS DONALD ALFRED; ATHERTON ERIC 权利人:AVECIA BIOLOG LTD 摘要:A process is provided for the solid-phase synthesis of a peptide amide which comprises attaching an α-nitrogen protected Cα-carboxamide amino acid to a solid support by its side chain, removing the α-nitrogen protecting group, assembling a peptide chain on said α-nitrogen and then cleaving the assembled peptide amide from the solid support. Novel amino acid analogues, peptide amides and solid-phase supports are also provided.
专利号:US-4131521-A 优先权日:1977-11-07 标题 :Electrochemical synthesis of organic carbonates 发明人:CIPRIS DIVNA; MADOR IRVING L 权利人:ALLIED CHEM 摘要:A process is described for the electrochemical synthesis of organic carbonates, such as dimethyl carbonate and ethylene carbonate, useful as industrial solvents for polymers and resins, which comprises electrolyzing a liquid medium containing a nonfluoride halide-containing electrolyte and a paraffinic monohydric or 1,2-dihydric alcohol. The non-fluoride halide-containing electrolyte is present in an amount of about 0.01 to 10 weight percent of the alcohol used, and the electrolysis is conducted by passing a direct current through the liquid medium at a temperature below its boiling point and under a carbon monoxide atmosphere at a pressure of about 1 to 350 atmospheres.
[参考文献]: A Soltan Monem, Et Al. Mesoporous Silica Coated Gold Nanorods Loaded Doxorubicin For Combined Chemo-Photothermal Therapy. Int J Pharm. 2014 Aug 15;470(1-2):1-7. [参考文献]: Ali Akbar Asgharinezhad, Et Al. Dispersive Micro-Solid-Phase Extraction Of Benzodiazepines From Biological Fluids Based On Polyaniline/magnetic Nanoparticles Composite. Anal Chim Acta. 2014 Sep 24:844:80-9. [参考文献]: Gulnara A Gainanova, Et Al. Self-Assembling Systems Based On Amphiphilic Alkyltriphenylphosphonium Bromides: Elucidation Of The Role Of Head Group. J Colloid Interface Sci. 2012 Feb 1;367(1):327-36. [参考文献]: K Rama Satyanarayana Raju, Et Al. 5-Aminosalicylic Acid Attenuates Allergen-Induced Airway Inflammation And Oxidative Stress In Asthma. Pulm Pharmacol Ther. 2014 Dec;29(2):209-16. [参考文献]: L Cheng, Et Al. Lipocalin-2 Promotes M1 Macrophages Polarization In A Mouse Cardiac Ischaemia-Reperfusion Injury Model. Scand J Immunol. 2015 Jan;81(1):31-8.
合成参考文献
参考文献:10.1007/bf00246709 摘要:ENGELHARDT A, JERCHEL D, WEIDMANN H, WICK H. [Synthesis, distribution and excretion of C14-marked 2-phenyl-3-methyl-tetrahydro-1, 4-oxazin (Preludin)]. Naunyn Schmiedebergs Arch Exp Pathol Pharmakol. 1958;235(1):10–8.