合成目标产物 Ethyl Chloroacetate 主要起始原料 Ethanol And Chloroacetic Acid
(文献来源)合成步骤主要原料 Ethanol 和 Chloroacetic Acid
乙酰乙酸乙酯置于potassium Bromate,盐酸体系中,用 N,N-二甲基甲酰胺 用作溶剂,化学反应 12.0H,以63%的收率获得氯乙酸乙酯 参考文献:Chlorinating Properties Of The Trimethylchlorosilane-Potassium Bromate-Dmf System 标题:Chlorinating Properties Of The Trimethylchlorosilane-Potassium Bromate-Dmf System 摘要:Beta-Dicarbonyl Compounds Such As Ethyl Acetoacetate,Dimedone,And Meldrum'S Acid Derivatives Undergo Monochlorination By The Action Of A Mixture Of Clsime3 And Kbro3 In Dmf At Approximately 20-Degrees-C. Doi:10.1007/bf00869533
专利号:WO-2004037772-A1 优先权日:2002-10-22 标 题 :Convenient and scalable synthesis of ethyl n-[(2-boc-amino) ethyl] glycinate and its hydrochloride salt 发明人:HUDSON ROBERT H E; VIIRRE RUSSELL D 权利人:UNIV WESTERN ONTARIO; HUDSON ROBERT H E; VIIRRE RUSSELL D 摘要:The present invention discloses an improved synthesis of ethyl N-[(2-Boc-amino)ethyl]glycinate and its hydrochloride salt. The synthesis is based on the reductive alkylation of Boc-ethylenediamine with ethyl glyoxylate hydrate and furnishes the title compound in near quantitative yield and high purity without chromatography. This compound is suitable, as is, for the synthesis peptide nucleic acid monomers. Further, conversion to the hydrochloride salt provides a stable, non-hygroscopic solid that is a convenient form for handling and storage.
专利号:US-4379935-A 优先权日:1980-08-04 标 题 :Process for the synthesis of vincamine and related indole alkaloids 发明人:PARACCHINI SILVANO; MORA PAOLO C 权利人:CORVI MORA PAOLO 摘要:A process is taught for the synthesis of vincamine and related indole alkaloids, according to which, through only two steps and through a novel synthesis intermediate, namely the glycidic ester, having the formula ##STR1## wherein R' represents --COOCH 3 or --COOCH 2 CH 3 , 1-ethyl-1,2,3,4,5,6,7,12b-octahydroindole[2,3-a]quinolizine-1-carboxaldehyde is reacted with a haloester in the presence of a base and the glycidic ester is converted to vincamine or apovincamine or like esters by reaction with a Lewis acid or a mineral acid, the reaction products being subsequently separated by chromatography.
专利号:US-5057624-A 优先权日:1989-03-31 标 题 :Process for the synthesis of the n-methyl-3,4-dimethoxyphenylethylamine 发明人:CANNATA VINCENZO; TAMERLANI GIANCARLO; ZAGNONI GRAZIANO 权利人:ALFA WASSERMANN SPA 摘要:New process for the synthesis of the N-methyl-3,4-dimetoxyphenylethylamine of formula ##STR1## intermediate in the synthesis of the drug internationally known as verapamil. The process starts from the 3,4-dimethoxybenzaldehyde which, by means of a Darzens condensation, gives an epoxyester that, by alkaline hydrolysis and subsequent decarboxylation, gives the 3,4-dimethoxyphenylacetaldehyde. This aldehyde gives the amine of formula I by reaction with monomethylamine followed by reduction with sodium borohydride.
专利号:US-5097058-A 优先权日:1987-04-08 标题:Process for the synthesis of the α-(-methyl-ethyl)-3,4-dimethoxybenzene-acetonitrile 发明人:CANNATA VINCENZO; TAMERLANI GIANCARLO; ZAGNONI GRAZIANO 权利人:ALFA WASSERMANN SPA 摘要:New process for the synthesis of the α-(1-m.ethylethyl)-3,4-dimethoxyacetonitrile of formula (I): ##STR1## which is known as an intermediate in the synthesis of the drug internationally known as verapamil. The process starts from the isobutyryl-3,4-dimethoxybenzene of formula (II): ##STR2## which, by means of the Darzens condensation, gives an epoxyester which, by alkaline hydrolysis and subsequent decarboxylation, gives the α-(1-methylethyl)-3,4-dimethoxybenzeneacetaldehyde. This product is reacted with hydroxylamine to obtain the corresponding oxime that, by dehydration, gives the nitrile of formula I.
专利号:WO-2012059797-A1 优先权日:2010-11-04 标题 :Process for synthesis of (s) - pregabalin 发明人:ROY BHAIRAB NATH; SINGH GIRIJ PAL; LATHI PIYUSH SURESH; AGRAWAL MANOJ KUNJABIHARI; MITRA RANGAN; RUPNAWAR MANOJ DATTATRAYA 权利人:LUPIN LTD; ROY BHAIRAB NATH; SINGH GIRIJ PAL; LATHI PIYUSH SURESH; AGRAWAL MANOJ KUNJABIHARI; MITRA RANGAN; RUPNAWAR MANOJ DATTATRAYA 摘要:Improved process for the synthesis of (S)-pregabalin having more than 99% ee through (S) 3-cyano-5-methyl-hexanoic acid has been developed. In addition to above, a novel process for resolution of ( RS ) - 3-cyano-5-methyl-hexanoic acid through diastereomeric salt formation with cinchonidine to obtain ( S ) - 3-cyano-5-methyl-hexanoic acid in high yield and high optical purity has been developed and furthermore process for recovery/ reuse of cinchonidine is also developed to improve the overall process efficiency.
专利号:US-11028057-B2 优先权日:2018-02-28 标题:Process for the synthesis of 6-chloromethyluracil 发明人:MORANA FABIO; GOBBATO STEFANO; ROLETTO JACOPO; PAISSONI PAOLO 权利人:PROCOS SPA 摘要:The invention relates to a process for the synthesis of 6-chloromethyluracil (6-(chloromethyl)pyrimidin-2,4(1H,3H)-dione) from ethyl 4-chloroacetoacetate and S-methylisothiourea hemisulfate via isolation of the novel intermediate 6-(chloromethyl)-6-hydroxy-2-(methylthio)-5,6-dihydropyrimidin-4(1H)-one, and its subsequent treatment with aqueous sulfuric acid. Formula (I).
参考标题:Design, Synthesis And Biological Evaluation Of Novel Quinazoline-2,4-Diones Conjugated With Different Amino Acids As Potential Chitin Synthase Inhibitors 作者:Nada A. Noureldin,Hend Kothayer,El-Sayed M. Lashine,Mohamed M. Baraka,Yanrong Huang,Bing Li,Qinggang Ji |发布日期:2018.5 摘要:Acetamido) Acids) (6 A-M), (7) Has Been Designed To Inhibit The Action Of Fungus Chitin Synthase Enzyme (Chs). The Synthesis Of The Designed Compounds Was Carried Out In Four Steps Starting From The Reaction Between 1-Methylquinazoline-2,4(1H,3H)-Dione And Ethyl Chloroacetate To Yield The Ethyl Acetate Derivative. This Ester Was Hydrolyzed To The Corresponding Carboxylic Acid Derivative That Was Then
合成参考文献
摘要:Stanforth, S. P., Science of Synthesis Knowledge Updates, (2014) 3, 105. 摘要:Kwiecień, H., Science of Synthesis Knowledge Updates, (2014) 4, 103. 摘要:Sainsbury, M., Science of Synthesis Knowledge Updates, (2010) 1, 261. 摘要:Podlech, J., Science of Synthesis Knowledge Updates, (2019) 1, 377. 摘要:Aggarwal, P.; Bebbington, M. W. P., Science of Synthesis Knowledge Updates, (2012) 2, 369.