N,O-双三甲硅基乙酰胺,N-甲基-2,2,2-三氟乙酰胺 以 苯 用作溶剂,化学反应 3.0H,反应生成N-甲基-N-(三甲基硅烷基)三氟乙酰胺 参考文献:N-메틸-N-트리메틸실릴 트리플루오로아세트아미드의 합성 방법,이로부터 합성된 N-메틸-N-트리메틸실릴 트리플루오로아세트아미드 및 이를 포함하는 리튬 이차전지용 전해액 标题:N-메틸-N-트리메틸실릴 트리플루오로아세트아미드의 합성 방법,이로부터 합성된 N-메틸-N-트리메틸실릴 트리플루오로아세트아미드 및 이를 포함하는 리튬 이차전지용 전해액 摘要:这项发明涉及一种n-甲基-N-三甲基硅基三氟乙酰胺(n-Methyl-N-Trimethylsilyl Trifluoroacetamide)(mstfa)的合成方法,由此合成的mstfa,以及包含它的锂二次电池电解液.该发明涉及使用三氟乙酸乙酯(ethyltrifluoroacetate)和甲胺(methylamine)制备n-甲基三氟乙酰胺(n-Methyltrifluoroacetamide)的步骤,以及将三甲基氯硅烷(trimethylsilyl Chloride)加入到n-甲基三氟乙酰胺(n-Methyltrifluoroacetamide)和三乙胺(triethylamine)混合物中,从反应混合物中分离沉淀物以获得mstfa的步骤.根据本发明,可以通过分馏来相对容易地去除未反应的起始物质和副反应物,从而获得99.0%以上的高纯度mstfa,并且当将99.0%以上的高纯度mstfa用作锂二次电池电解液的添加剂时,可以提高锂二次电池的寿命特性.
专利号:WO-9741093-A1 优先权日:1996-04-30 标 题:Methods for the synthesis of fmoc protected amines 发明人:BAER TED ALLEN; RAILLARD STEPHEN PETER 权利人:AFFYMAX TECH NV; BAER TED ALLEN; RAILLARD STEPHEN PETER 摘要:Methods for the synthesis of Fmoc-protected amines are provided. These methods involve the treatment of an amine component with a silylating agent and then an activated Fmoc-reagent. The methods can be conducted under anhydrous conditions.
专利号:US-9873905-B2 优先权日:2014-03-07 标题:Chemoenzymatic synthesis of trehalose analogs 发明人:SWARTS BENJAMIN M; WOODRUFF PETER 权利人:CENTRAL MICHIGAN UNIV; UNIV OF MAINE SYSTEM 摘要:The present invention provides methods of synthesizing trehalose analogs; methods of detecting mycobacteria, and trehalose analogs.
专利号:US-7279605-B2 优先权日:2004-11-11 标 题:Synthesis of cyclopentenones 发明人:JACOBY DENIS; KELLER FABRICE 权利人:FIRMENICH & CIE 摘要:The invention relates to a process for the preparation, in a single step, of substituted 2-cyclopenten-1-ones by reacting a substituted enone with an aldehyde in the presence of a catalytic system. The catalytic system consists of a metal complex, such as a Ti(Cl) 3 (alkoxy), and a co-ingredient, such as a carboxylic acid anhydride or an anhydrous salt.
专利号:US-2007004929-A1 优先权日:2005-06-29 标题 :Synthesis of labeled compounds 发明人:MARTINEZ RODOLFO A; SCHMIDT JURGEN G; ALVAREZ MARC A; SILKS LOUIS A 权利人:MARTINEZ RODOLFO A; SCHMIDT JURGEN G; ALVAREZ MARC A; SILKS LOUIS A 摘要:The present invention is directed to labeled compounds of the formula Ar-Z 1 -Q-Z 2 where Ar is an aryl group is selected from the group consisting of 1-naphthyl, substituted 1-naphthyl, 2-naphthyl, substituted 2-naphthyl, and phenyl groups with the structure n n nwherein R 1 , R 2 , R 3 , R 4 and R 5 are each independently selected from the group consisting of hydrogen, a C 1 -C 4 lower alkyl, a halogen, a phenyl, an alkoxy group and an amino group from the group consisting of NH 2 , NHR and NRR′ where R and R′ are each a C 1 -C 4 lower alkyl, Q is selected from the group consisting of 13 CH 2 , 13 CDH and 13 CD 2 , and Z 1 is selected from the group consisting of —S—, —S(â•?O)—, —S(â•?O) 2 —, —Se—, —Se(â•?O)—, and —Se(â•?O) 2 —, Z 2 is selected from the group consisting of —Si(R 6 R 7 R 8 ), —O(R 9 ), —Se—Ar, —Se(â•?O)—Ar, —Se(â•?O) 2 —Ar, —S—Ar, —S(â•?O)—Ar, and —S(â•?O) 2 —Ar wherein R 6 , R 7 and R 8 are each independentl selected from the group consisting of a C 1 -C 4 lower alkyl, R 9 is a C 1 -C 4 lower alkyl or an R 10 —Ar group where R 10 is a C 1 -C 4 alkylene group.
专利号:US-9605019-B2 优先权日:2011-07-19 标 题:Methods for the synthesis of functionalized nucleic acids 发明人:VERDINE GREGORY L; MEENA; IWAMOTO NAOKI; BUTLER DAVID CHARLES DONNELL 权利人:VERDINE GREGORY L; MEENA; IWAMOTO NAOKI; BUTLER DAVID CHARLES DONNELL; WAVE LIFE SCIENCES LTD 摘要:The present application, among other things, provides technologies, e.g., reagents, methods, etc. for preparing oligonucleotides comprising phosphorothiotriesters linkages, e.g., oligonucleotides having the structure of IIIa, IIIb or IIIc. In some embodiments, provided methods comprise reacting an H-phosphonate of structure Ia or Ib with a silylating reagent to provide a silyloxyphosphonate, and reacting the silyloxyphosphonate with a thiosulfonate reagent of structure IIa or IIb to provide an oligonucleotide of structure IIIa or IIIb. In some embodiments, provided methods comprise reacting an H-phosphonate of structure Ic with a silylating reagent to provide a silyloxyphosphonate, reacting the silyloxyphosphonate with a bis(thiosulfonate) reagent of structure IVc to provide a phosphorothiotriester comprising a thiosulfonate group of structure Vc, and then reacting the phosphorothiotriester comprising a thiosulfonate group of structure Vc with a nucleophile of structure VIc to provide an oligonucleotide of structure IIIc.
专利号:US-9309547-B2 优先权日:2012-05-22 标题:Methods for making tocoflexols and analogues thereof 发明人:ZHENG GUANGRONG; COMPADRE CESAR; HAUER-JENSEN MARTIN; CROOKS PETER; BREEN PHILIP 权利人:UNIV ARKANSAS; US DEPT VETERANS AFFAIRS; US OF AMERICA AS REPRESENTED BY THE DEPT OF VETERANS AFFAIRS 摘要:Methods for the synthesis of tocoflexols of Formula (I) and (II) and a number of related tocol analogs are provided herein. The methods are economical and amenable to large scale production and can be performed using either pure of partially purified tocotrienols as the starting material.
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合成参考文献
参考文献:10.1007/s00216-010-3479-0 摘要:Wagner BM, Donnarumma F, Wintersteiger R, Windischhofer W, Leis HJ. Simultaneous quantitative determination of α-ketoglutaric acid and 5-hydroxymethylfurfural in human plasma by gas chromatography–mass spectrometry. Analytical and Bioanalytical Chemistry. 2010 Feb 14;396(7):2629–37. doi: 10.1007/s00216-010-3479-0. 参考文献:10.1016/j.mimet.2011.07.001 摘要:Marcinowska R, Trygg J, Wolf-Watz H, Mortiz T, Surowiec I. Optimization of a sample preparation method for the metabolomic analysis of clinically relevant bacteria. J Microbiol Methods. 2011 Oct;87(1):24–31. doi: 10.1016/j.mimet.2011.07.001.