D-葡萄糖置于三氯化铝,Trioxane体系中,用 甲醇 作为反应溶剂,化学反应生成 α-乙酰基-γ-丁内酯 参考文献:Selective Dehydration Of Glucose To Hydroxymethylfurfural And A One-Pot Synthesis Of A 4-Acetylbutyrolactone From Glucose And Trioxane In Solutions Of Aluminium Salts 标题:Selective Dehydration Of Glucose To Hydroxymethylfurfural And A One-Pot Synthesis Of A 4-Acetylbutyrolactone From Glucose And Trioxane In Solutions Of Aluminium Salts 摘要:Saturated Water Solutions Of Al-2(So4)(3) And Alcl3 Were Applied As Solvent:Matrices For Dehydration Of Glc To Hydroxymethylfurfural (Hmf). Addition Of Oxygen Ligands: Methanol,Ethanol,Thf,Furan,Dibutyl Ether,Ethyl Orthoformate And Trioxane Influenced The Yield And Selectivity,The Best Being Observed With Ethanol. When Glc And Trioxane Were Present Together In Reacting Solution,Formation Of A 4-Acetylbucyrolactune Was Observed. (C) 1999 Elsevier Science Ltd. All Rights Reserved. DOI:10.1016/s0008-6215(99)00037-3
专利号:US-7977480-B2 优先权日:2007-12-10 标 题:Synthesis of paliperidone 发明人:BARTL JIRI; KRAJCOVIC JOZEF; BENOVSKY PETR 权利人:SYNTHON BV 摘要:A 9-hydroxy or 9-acyloxy group can be added to a pyridopyrimidinone ring structure by a process comprising acylating a compound of formula (5) under Vilsmeier-Haack or Friedel-Crafts conditions to form a compound (6); and transforming with a peroxo-compound to obtain the compound (1). n nR represents hydrogen or a C1-C20 acyl group. The process is useful in the synthesis of paliperidone and derivatives.
专利号:US-12071410-B2 优先权日:2018-02-26 标 题:High-yielding continuous flow synthesis of antimalarial drug hydroxychloroquine 发明人:GUPTON FRANK B; AHMAD SAEED; GUNURU HARI P R; TELANG NAKUL S 权利人:UNIV VIRGINIA COMMONWEALTH 摘要:Cost effective, semi-continuous flow methods and systems for synthesizing the antimalarial drug hydroxychloroquine (HCQ) in high yield are provided. The synthesis method that uses simple, inexpensive reagents to obtain the crucial intermediate 5-(ethyl(2-hydroxyethyl)-amino)pentan-2-one, vertical-integration of the starting material 5-iodopentan-2-one and the integration of continuous stirred tank reactors.
专利号:US-2024425890-A1 优先权日:2022-02-11 标 题:Process for the synthesis of alpha-methylene-gamma-butyrolactone 发明人:TADEN ANDREAS; BECK HORST; MYRTOLLARI KAMELA; KOURIST ROBERT; NIGL ANDREA 权利人:HENKEL AG & CO KGAA 摘要:The present application provides a process for the preparation of α-methylene-γ-butyrolactone, said process comprising the steps of:a) acetylating the C1-hydroxyl group of isoprenol to yield isoprenyl acetate;b) forming 4-acetoxy-2-methylene-butan-1-ol from said isoprenyl acetate by whole cell biotransformation, said step comprising:i) contacting a cell (CB) with a culture medium containing said isoprenyl acetate or with a culture medium contiguous with an organic phase containing said isoprenyl acetate under conditions that enable the cell to form 4-acetoxy-2-methylene-butan-1-ol from isoprenyl acetate; and,ii) optionally isolating the resultant 4-acetoxy-2-methylene-butan-1-ol, wherein said cell (CB) exhibits activity of at least one alkane monooxygenase enzyme which catalyzes the formation of 4-acetoxy-2-methylene-butan-1-ol from isoprenyl acetate;c) oxidizing said 4-acetoxy-2-methylene-butan-1-ol to yield 4-acetoxy-2-methylene butyric acid; and,d) converting said 4-acetoxy-2-methylene butyric acid to α-methylene-γ-butyrolactone by hydroxylysis to γ-hydroxy-α-methylenebutyric acid and subsequent cyclization of said γ-hydroxy-α-methylenebutyric acid.
专利号:US-7371769-B2 优先权日:2004-12-07 标 题 :Tetrahydropyridin-4-yl indoles with a combination of affinity for dopamine-D2 receptors and serotonin reuptake sites 发明人:HES ROELOF VAN; SMID PIETER; KRUSE CORNELIS G; TULP MARTINUS TH M 权利人:SOLVAY PHARM BV 摘要:The present invention relates to a group of novel tetrahydropyridin-4-yl indoles with a dual mode of action: serotonin reuptake inhibition and affinity for dopamine-D 2 receptors, to methods for the preparation of these compounds and to novel intermediates useful for the synthesis of said tetrahydropyridin-4-yl indoles. The invention also relates to the use of a compound disclosed herein for the manufacture of a medicament giving a beneficial effect. n The invention relates to novel tetrahydropyridin-4-yl indoles of the formula. n nand tautomers, stereoisomers, prodrugs, N-oxides, pharmacologically acceptable salts, hydrates and solvates thereof,n nwherein:n R 1 is hydrogen, halogen, alkyl(C 1-3 ) or alkoxy(C 1-3 ), CN or CF 3 , R 2 is hydrogen or alkyl(C 1-3 ), R 3 is hydrogen or alkyl(C 1-3 ), Z is hydrogen or alkyl(C 1-3 ), alkoxy(C 1-3 ) or alkylthio(C 1-3 ), A is hydrogen or alkyl(C 1-3 ), or A and Z together form a saturated or (partly) unsaturated 5- or 6-membered ring which may be substituted with halogen, alkyl (C 1-3 ) or phenyl, in which ring Z represents carbon, sulfur of nitrogen.
专利号:US-8309695-B2 优先权日:2007-06-11 标题 :Marking reagents bearing diazo and nitro functions, methods for the synthesis of such reagents and methods for detecting biological molecules 发明人:LAURENT ALAIN; LAAYOUN ALI; KOTERA MITSUHARU 权利人:LAURENT ALAIN; LAAYOUN ALI; KOTERA MITSUHARU; BIOMERIEUX SA; CENTRE NAT RECH SCIENT; UNIV STRASBOURG 摘要:The present invention relates to a labeling reagent of formula: n nin which:n R 1 represents at least one detectable label, L and A are each a linker arm, n is an integer equal to 1, and u is an integer between 0 and 2.n nThe present invention also describes a method of synthesizing said markers and also applications for the labeling of biological molecules, more particularly nucleic acids, with a labeling reagent bearing diazo and nitro functions. The invention is particularly suitable for use in the diagnostics field.
专利号:US-2008214809-A1 优先权日:2006-08-23 标 题 :Process for the synthesis of CMHTP and intermediates thereof 发明人:DOLITZKY BEN-ZION; SHAPIRO EVGENY; INI SANTIAGO; SHMUELY YARON; LANCRY ELI; PILARSKY GIDEON 权利人:DOLITZKY BEN-ZION; SHAPIRO EVGENY; INI SANTIAGO; SHMUELY YARON; LANCRY ELI; PILARSKY GIDEON 摘要:The present invention provides processes of preparing 3-(2-chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrrido[1,2-a]-pyrimidin-4-one (CMHTP) useful as intermediates for the preparation of paliperidone, wherein the processes use 3-(2-chloroethyl)-2-methyl-9-benzyloxy-4H-pyrido[1,2-a]pyrimidine-4-one (CMBP) and/or 3-(2-chloroethyl)-2-methyl-9-hydroxy-4H-pyrido[1,2-a]pyrimidine-4-one (CMHP) having phosphorus at least partially removed as the intermediate.