三溴甲烷置于甲醇,Sodium体系中,化学反应 4.0H,以100%的收率获得原甲酸三甲酯 参考文献:Electrocchemicai Oxidatiob Of Ketones In Methanol In The Presence Of Alkali Metal Bromides 标题:Electrocchemicai Oxidatiob Of Ketones In Methanol In The Presence Of Alkali Metal Bromides 摘要:Electrochemical Oxidation Of Methyl Ketones In Methanol In The Presence Of Alkali Metal Bromides Affords Methyl Carboxylates. Benzyl Alkyl Ketones Are Transformed Under Similar Conditions Into Methyl 3-Phenylalkanoates,While Ketones Lacking Alpha-Benzyl Or Alpha-Methyl Group Are Oxidized Into Alpha-Hydroxyketals. Doi:10.1016/s0040-4020(01)87078-2
专利号:US-7247752-B2 优先权日:2004-10-01 标 题 :Methods for the synthesis of astaxanthin 发明人:LOCKWOOD SAMUEL F; TANG PENG CHO; NADOLSKI GEOFF; JACKSON HENRY L; FANG ZHIQIANG; DU YISHU; YANG MIN; GEISS WILLIAM; WILLIAMS RICHARD; BURDICK DAVID 权利人:CARDAX PHARMACEUTICALS INC 摘要:A method used for synthesizing intermediates for use in the synthesis of carotenoids and carotenoid analogs, and/or carotenoid derivatives. In some embodiments, the invention includes methods for synthesizing optically active intermediates useful for the synthesis of optically active carotenoids. Synthesis of optically active carotenoids, in one embodiment, may be accomplished by forming an optically active dihydroxy intermediate from ketoisopherone. The optically active dihydroxy intermediate may be converted into optically active astaxanthin derivatives.
专利号:WO-9740025-A1 优先权日:1996-04-19 标 题 :Solid phase and combinatorial synthesis of substituted 1,2,3-triazoles and of arrays of substituted 1,2,3-triazoles 发明人:DOERWALD FLORENCIO ZARAGOZA 权利人:NOVO NORDISK AS; DOERWALD FLORENCIO ZARAGOZA 摘要:A solid phase method for the synthesis of a plurality of differently substituted 1,2,3-triazoles with a wide variety of side-chain substituents as compounds of potential therapeutic interest. The 1,2,3-triazoles are prepared by acylation of a substrate-bound primary or secondary amine with a 3-oxoalkanoic acid and reaction of the resulting amide with a primary amine under dehydrating conditions to give an enamine. Treatment of this substrate-bound enamine with a sulfonyl azide in the presence of a base gives the corresponding 1,2,3-triazoles. These may be screened on the substrate or cleaved from the substrate and then screened in solution. The efficient synthesis of a wide variety of 1,2,3-triazoles using automated synthesis technology of the present method makes these compounds attractive candidates for the generation and rapid screening of diverse triazole-based libraries. The method disclosed here provides an easy and fast access to highly diverse heterocyclic compounds of therapeutic interest, amenable to automatization.
专利号:US-6251689-B1 优先权日:1998-05-14 标 题:Methods for the solid phase synthesis of combinatorial libraries of benzimidazoles benzoxazoles benzothiazoles and derivatives thereof 发明人:LABORDE EDGARDO; MATSUMOTO YUKIHARU 权利人:TELIK INC 摘要:The present invention provides an efficient and versatile method for the synthesis and screening of combinatorial libraries of benzimidazoles, benzoxazoles, benzothiazoles, and derivatives thereof. In order to expedite the synthesis of large arrays of compounds possessing these core structures, a general methodology for solid phase synthesis of these derivatives is provided. Arrays of benzimidazoles, benzoxazoles, benzothiazoles, and derivatives thereof useful as peptidomimetics and for the identification of agents having antifungal, antiviral, antimicrobial, anticoagulant, and antiulcer activity, or use in the treatment of inflammation, hypertension, cancer, and other conditions can be prepared by this method.
专利号:US-5668285-A 优先权日:1986-10-31 标 题 :Total synthesis of northebaine, normophine, noroxymorphone enantiomers and derivatives via N-Nor intermediates 发明人:RICE KENNER CRALLE; NEWMAN AMY HAUCK 权利人:US HEALTH 摘要:The invention involves a method of making key intermediates useful in the synthesis of many opiate narcotics and antagonists and agonists; and the non-opiate enantiomers thereof which have potent antitussive properties. The synthesis starts from either the natural or unnatural enantiomer of nordihydrocodeinone and produces 8, 14-dihydronorthebaine, the diketal of 7-bromonordihydrocodeinone, northebaine, norcodeinone diketal and 14-hydroxynorcodeinone intermediates without the necessity of leaving the N-nor structure. The syntheses have fewer steps than previous methods, and also have high yields.
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-7714063-B2 优先权日:2007-11-15 标 题 :Solid support for Fmoc-solid phase synthesis of peptides 发明人:SRIVASTAVA KRIPA SHANKER; DAVIS MATTHEW RYAN 权利人:MALLINCKRODT INC 摘要:The present invention provides compositions and processes for the solid phase synthesis of polypeptides. In particular, the present invention provides solid supports and processes for preparing solid supports for the synthesis of polypeptides.
摘要:Kostikov, R. R.; Khlebnikov, A. F.; Sokolov, V. V., Science of Synthesis, (2010) 47, 851. 摘要:Chciuk, T. V.; Flowers, R. A.; Flowers, R. A., Science of Synthesis Knowledge Updates, (2016) 2, 184. 摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2010) 2, 176. 摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2018) 2, 215. 摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2018) 2, 88.