N-甲基二乙醇胺置于rare-Earth Based Solid Catalyst体系中,化学反应生成N-甲基吗啉 参考文献:一种催化制备n-甲基吗啉的方法 标题:一种催化制备n-甲基吗啉的方法 摘要:本发明公开了一种催化制备n‑甲基吗啉的方法,包括如下所述的制备步骤:步骤s1,将稀土基固体催化剂装填于管式反应器中;步骤s2,将液体原料n‑甲基二乙醇胺置于原料罐中,利用进样泵匀速进样,原料液通过管式反应器中的稀土基固体催化剂进行分子内脱水反应,原料液的液体体积空速为0.1‑0.5H‑1,反应器温度为200‑300oc;步骤s3,通过冷凝器冷凝收集步骤s2所得反应液,加入片碱使反应液分层,取上层液体进行常压精馏,收集115‑116oc馏分,得目标产物n‑甲基吗啉.本发明提供的方法简易可行,转化率高,催化剂可以反复使用,且反复使用六十次后催化效率无明显降低.
专利信息
专利号:US-8138330-B2 优先权日:2006-09-11 标 题 :Process for the synthesis of oligonucleotides 发明人:LEUCK MICHAEL; WOLTER ANDREAS; STUMPE ALFRED 权利人:LEUCK MICHAEL; WOLTER ANDREAS; STUMPE ALFRED; SIGMA ALDRICH CO LLC 摘要:The present invention discloses novel methods for the synthesis of oligonucleotides with nucleoside phosphoramidites on solid supports. The methods comprise the stepwise chain assembly of oligonucleotides on supports with 5′-acyl phosphoramidites. The synthesis cycles consist of a front end deprotection step which is conducted with a solution of a primary amine or a phenolate, a phosphoramidite coupling step with a 5′-acyl nucleoside phosphoramidite in the presence of an activator, a phosphite oxidation step and an optional capping step. The novel methods improve the quality of synthetic oligonucleotides due to the irreversibility of the front end deprotection step, which prevents the formation of deletion sequences, and due to the avoidance of acidic reagents in the synthesis cycles, which prevent the formation of depurination side products. The invention further discloses novel nucleoside phosphoramidite compositions wherein the phosphoramidites carry acyl front end protective groups which are cleavable with primary amines or phenolates. The invention is applicable to the synthesis of oligodeoxyribonucleotides, oligoribonucleotides and oligonucleotides with modifications in their sugar or phosphate groups.
专利号:WO-2023030277-A1 优先权日:2021-08-30 标 题:Method for fully liquid-phase synthesis of grnh nonapeptide amide analog 发明人:SUN PENGCHENG; PAN JING; WU JUNYONG; TANG YONGBO; Du Yixiong; GUO LIN 权利人:HUNAN MICRO PEPTIDE BIOMEDICAL CO LTD 摘要:Provided is a method for fully liquid-phase synthesis of a GRnH nonapeptide amide analog, which belongs to the technical field of medicine synthesis. The method comprises respectively synthesizing a 'Trp-Ser-Tyr' fragment, an 'R-Leu' fragment, a 'Pyr-His' fragment and 'Arg-Pro-Hunan T', wherein, R = D-Ala (alarelin), D-Leu (leuprorelin), D-Trp (deslorelin) and D-His (histrelin), and obtaining the GRnH nonapeptide amide analog with high yield and high purity by means of a '3 +2 +2 +2' fragment condensation method. The synthesis method is environmentally friendly, mild, and free of any highly toxic and poisonable reagents. The cost is greatly reduced and the synthesis method is very suitable for large-scale production.
专利号:WO-2022256490-A9 优先权日:2021-06-03 标题:Improved synthesis of phosphoramidates for the treatment of hepatitis b virus 发明人:LOCKWOOD MARK 权利人:ANTIOS THERAPEUTICS INC 摘要:The synthesis of phosphoramidate prodrugs useful in the treatment of viral infections is disclosed. Specifically, an improved synthesis of phosphoramidate nucleotides useful in the treatment of Hepatitis B virus is disclosed.
专利号:US-2004242897-A1 优先权日:2002-07-31 标题 :Universal support media for synthesis of oligomeric compounds 发明人:GUZAEV ANDREI P; MANOHARAN MUTHIAH 摘要:Compounds for the synthesis of oligomeric compounds, particularly oligonucleotides and oligonucleotide mimetics, are provided. In addition, methods for functionalizing a support medium with a first monomeric subunit and methods for the synthesis of oligomeric compounds utilizing the novel compounds bound to support media are provided.
专利号:US-9994526-B2 优先权日:2011-04-04 标 题 :Process intermediates and methods for the preparation of process intermediates for the synthesis of argatroban monohydrate 发明人:STIVANELLO MARIANO; HUBER FLORIAN ANTON MARTIN; RICCI ANTONIO 权利人:LUNDBECK PHARMACEUTICALS ITALY S P A 摘要:Methods are provided for the synthesis of key intermediates for the synthesis of Argatroban monohydrate, ethyl (2R,4R)-1-[(2S)-2-amino-5-[[imino(nitroamino)methyl]amino]-1-oxopentyl]-4-methylpiperidine-2-carboxylate compounded with HCl. Such intermediates are also provided.
专利号:US-2006264608-A1 优先权日:2001-08-03 标题 :Bi-directional synthesis of oligoguanidine transport agents 发明人:WENDER PAUL A; VANDEUSEN CHRISTOPHER L; PATTABIRAMAN KANAKA; PELKEY ERIN T; JESSOP THEODORE C 权利人:WENDER PAUL A; VANDEUSEN CHRISTOPHER L; PATTABIRAMAN KANAKA; PELKEY ERIN T; JESSOP THEODORE C 摘要:Synthesis routes that can be adapted to large scale synthesis of oligoguanidine compounds such as oligoarginine compounds are described which use a perguanidinylation step to convert a group of ω-amino groups to the corresponding guanidinyl groups. These compounds find utility as transport agents. Modified oligoguanidine compounds are also described.
参考文献:10.1007/978-1-61779-188-8_2 摘要:Gaynor JW, Cosstick R. Dinucleotides containing 3'-S-phosphorothiolate linkages. Methods Mol Biol. 2011;764():17–30. doi: 10.1007/978-1-61779-188-8_2. 参考文献:10.1107/s1600536811019295 摘要:Jing Y, Yu LT. 2-[4-(Diethyl-amino)-benzyl-idene]malono-nitrile. Acta Crystallogr Sect E Struct Rep Online. 2011 Jun 01;67(Pt 6):o1556. 参考文献:10.1074/jbc.m111.273722 摘要:Pedersen JW, Bennett EP, Schjoldager KT-G, Meldal M, Holmér AP, Blixt O, Cló E, Levery SB, Clausen H, Wandall HH. Lectin Domains of Polypeptide GalNAc Transferases Exhibit Glycopeptide Binding Specificity. Journal of Biological Chemistry. 2011 Sep;286(37):32684–96. doi: 10.1074/jbc.m111.273722. 参考文献:10.1016/j.forsciint.2011.06.030 摘要:McDermott SD, Power JD, Kavanagh P, O'Brien J. The analysis of substituted cathinones. Part 2: an investigation into the phenylacetone based isomers of 4-methylmethcathinone and N-ethylcathinone. Forensic Sci Int. 2011 Oct 10;212(1-3):13–21. doi: 10.1016/j.forsciint.2011.06.030. 参考文献:10.4061/2011/652702 摘要:Crawford MJ, Rapireddy S, Bahal R, Sacui I, Ly DH. Effect of Steric Constraint at the γ-Backbone Position on the Conformations and Hybridization Properties of PNAs. J Nucleic Acids. 2011;2011():652702.