对羟基苯甲醇置于iron(Iii) Chloride,2,2,6,6-四甲基哌啶氧化物,盐酸羟胺,碘,Potassium Carbonate体系中,用 1,2-二氯乙烷 作为反应溶剂,化学反应 16.0H,以80%的收率获得产物4-羟基苯甲酰胺 参考文献:I2-Tempo As An Efficient Oxidizing Agent For The One-Pot Conversion Of Alcohol To Amide Using Fecl3 As The Catalyst 标题:I2-Tempo As An Efficient Oxidizing Agent For The One-Pot Conversion Of Alcohol To Amide Using Fecl3 As The Catalyst 摘要:A High Yield One-Pot Method For The Synthesis Of Amides From Alcohols Is Described. The Aldehyde Was Generated In Situ Using Iodine-Tempo As Oxidizing Agent Followed By Intermediate Oxime Formation Through Reaction With Nh2Oh Center Dot Hcl And Finally Rearrangement Of Oxime Catalyzed By Fecl3. (C) 2012 Elsevier B.V. All Rights Reserved. DOI:10.1016/j.Catcom.2012.04.027
专利号:WO-9617589-A1 优先权日:1994-12-08 标 题 :Method of smoothing or removing wrinkles and method of stimulating collagen synthesis 发明人:FUJIMURA TSUTOMU; OGAWA AYUMI; OHSU HIROYUKI; TAKEMA YOSHINORI; HORI KIMIHIKO; AMANO SHINYA; FUJIMORI TAKETOSHI; OHASHI YUKIHIRO; SUZUKI YASUTO 权利人:KAO CORP; FUJIMURA TSUTOMU; OGAWA AYUMI; OHSU HIROYUKI; TAKEMA YOSHINORI; HORI KIMIHIKO; AMANO SHINYA; FUJIMORI TAKETOSHI; OHASHI YUKIHIRO; SUZUKI YASUTO 摘要:The present invention relates to methods of stimulating collagen synthesis and of smoothing or removing wrinkles, which comprise administering an effective amount of a benzoic acid derivative of formula (1) or a salt thereof, wherein X is -O- or -N(R4)- (R4 is H or the like), R1 is a C¿4-25?-alkyl or C4-25-alkenyl group, R?2¿ is H, OH, or a C¿1-6?-alkoxyl or C1-6-alkanoyloxy group, and R?3 is -OR5¿ or -N(R?6)R7 (R5? is H, or a C1-25-alkyl or C1-25-alkenyl group), and R?6 and R7¿ are individually H, or a C¿1-3?-alkyl or C1-3-alkenyl group, and use of this compound for agents for stimulating synthesis of collagen, and smoothing or removing wrinkles. This compound (1) stimulates collagen synthesis in human dermal fibroblasts and consequently smooths or removes wrinkles caused by aging and/or photoaging.
专利号:WO-2014087110-A1 优先权日:2012-12-07 标 题:Method for synthesising an addition salt with a pharmaceutically acceptable acid of 4-{3-[cis-hexahydrocyclopenta[c]pyrrol-2(1h)-yl]propoxy}benzamide, and the associated crystalline forms 发明人:PIERRY CAMILLE; ROBERT NICOLAS; LECOUVE JEAN-PIERRE; LETELLIER PHILIPPE 权利人:SERVIER LAB 摘要:A method for the industrial synthesis of an addition salt with a pharmaceutically acceptable acid of 4-{3-[ cis -hexahydrocyclopenta[ c ]pyrrol-2(1 H )-yl]propoxy}benzamide of formula (I), in which ΗΧ represents a pharmaceutically acceptable acid, and the associated crystalline forms. Drugs
专利号:US-5399757-A 优先权日:1993-07-20 标题 :Process for the preparation of N-(4-hydroxyphenyl)-retinamide 发明人:MARYANOFF CYNTHIA A 权利人:ORTHO PHARMA CORP 摘要:This invention is directed to an efficient, mild, high yield process for the large scale synthesis of N-(4-hydroxyphenyl)-retinamide comprising the preferred steps of reacting retinoic acid with dimethylchloroformamidinium chloride to from retinoyl chloride which in turn is reacted with bis-(N,O)-trimethylsilyl-p-aminophenol to eventually form N-(4-hydroxyphenyl)-retinamide and to the novel use of bis-(N,O)-trimethylsilyl-p-aminophenol to eventually form a hydroxyphenylamide, particularly N-(4-hydroxyphenylretinamide and methods of recrystallizing N-(4-hydroxyphenyl)-retinamide to obtain the stable 'A' polymorph thereof.
专利号:US-10807953-B2 优先权日:2015-03-02 标题:Processes and intermediates for the preparation of Pimavanserin 发明人:BILJAN TOMISLAV; DOGAN JASNA; METSGER LEONID; PIPERCIC SARA MORASI; RATKAJ MARINA; SKUGOR MAJA MATANOVIC; WANG YI 权利人:PLIVA HRVATSKA D O O 摘要:The present disclosure relates to novel, safe and efficient processes for the synthesis of Pimavanserin and salts thereof, as well as novel intermediates that can be used in these processes.
专利号:US-6417368-B1 优先权日:1998-03-13 标题:Amine derivative fixed to resin and method for synthesizing β-aminocarbonyl compound in a solid phase 发明人:KOBAYASHI SHU; AOKI YOJI 权利人:JAPAN SCIENCE & TECH CORP 摘要:The invention provides a resin-immobilized imine represented by the following formula: n n n P—Q—N—â•?CH—R   I n n n [in the formula, P represents the principal chain of a resin polymer; Q represents a substituted or unsubstituted hydrocarbon side chain or a substituted or unsubstituted hydrocarbon side chain with a heteroatom interposed therein; R represents a substituted or unsubstituted hydrocarbon group or heterocyclic group] and a resin-immobilized β-aminocarbonyl compound of the following formula: n which can be released as β-aminocarbonyl compound from the solid phase; and the invention also provide a resin-immobilized amine of the following formula: n n n —P—Q 1 —O—Q 2 —NH 2   III n n n [Q 1 and Q 2 independently represent a hydrocarbon chain such as arylene, alkylenearylene or arylenealkylene], which is essential for solid state synthesis; and the invention has enabled the solid state synthesis of ²-aminocarbonyl compound by the application of iminoaldol reaction.
专利号:US-8952179-B2 优先权日:2011-06-08 标 题:Synthesis process, and crystalline form of 4-{3-[cis-hexahydrocyclopenta[c]pyrrol-2(1H)-yl]propoxy} benzamide hydrochloride and pharmaceutical compositions containing it 发明人:ROBERT NICOLAS; LERESTIF JEAN-MICHEL; LECOUVE JEAN-PIERRE; GAILLARD MARINA; MEUNIER LOIC; LETELLIER PHILIPPE; BOIRET MATHIEU 权利人:SERVIER LAB; SERVIER LAB 摘要:Industrial synthesis process for the compound of formula (I):
[参考文献]: Habsah Mohamad, Et Al. Potential Secondary Metabolites From Marine Sponge Aaptos Aaptos For Atherosclerosis And Vibriosis Treatments. Natural Product Communications. 2017. 12(8):1227-1230. [参考文献]: Alex N Manin, Et Al. Cocrystal Screening Of Hydroxybenzamides With Benzoic Acid Derivatives: A Comparative Study Of Thermal And Solution-Based Methods. Eur J Pharm Sci. 2014 Dec 18:65:56-64. [参考文献]: Alex N Manin, Et Al. Influence Of Secondary Interactions On The Structure, Sublimation Thermodynamics, And Solubility Of Salicylate:4-Hydroxybenzamide Cocrystals. Combined Experimental And Theoretical Study. J Phys Chem B. 2015 Aug 20;119(33):10466-77. [参考文献]: Carlos E S Bernardes, Et Al. Energetics Of The O-H Bond And Of Intramolecular Hydrogen Bonding In Hoc6H4C(O)Y (Y = H, Ch3, Ch2Ch=ch2, C[参考文献]: G D Hartman, Et Al. Nonpeptide Glycoprotein Iib/iiia Inhibitors. 19. A New Design Paradigm Employing Linearly Minimized, Centrally Constrained, Exosite Inhibitors. Bioorg Med Chem Lett. 1999 Mar 22;9(6):863-8.
合成参考文献
摘要:Wu, X.-F., Science of Synthesis Knowledge Updates, (2014) 1, 302. 摘要:Glushkov, V. A.; Shklyaev, Yu. V., Science of Synthesis Knowledge Updates, (2018) 3, 254. 摘要:Harsanyi, A.; Sandford, G., Science of Synthesis Knowledge Updates, (2015) 1, 172. 摘要:González-Bello, C., Science of Synthesis Knowledge Updates, (2018) 1, 212. 摘要:S109 | PARCEDC | List of 7074 potential endocrine disrupting compounds (EDCs) by PARC T4.2 | DOI:10.5281/zenodo.10944198