专利号:US-9969823-B1 优先权日:2011-09-01 标题 :Synthesis and polymerization of vinyl triazolium ionic liquids 发明人:LUEBKE DAVID; NULWALA HUNAID; MATYJASZEWSKI KRZYSZTOF; ADZIMA BRIAN 权利人:US ENERGY; THE US DEPARTMENT OF ENERGY 摘要:Herein, we describe polymerized ionic liquids, demonstrate the synthesis of polymerized ionic liquids, and demonstrate the polymerization of triazolium monomers. One embodiment shows the polymeriazation of the triazolium monomers with bis(trifluoromethanesulfonyl)imide anions. In another embodiment we show the feasibility of copolymerizing with commodity monomers such as styrene using free radical polymerization techniques.
专利号:EP-1638988-B1 优先权日:2003-06-30 标题:Process for the synthesis of high purity d-(17alpha)-13-ethyl-17hydroxy-18,19-dinorpre:gn-4-ene-20-yne-3-one-oxime 发明人:TUBA ZOLTAN; MAHO SANDOR; KISS JANOS; MAGYARI ENDRENE; TERDY LASZLO 权利人:RICHTER GEDEON NYRT 摘要:The invention relates to a process for the synthesis of high purity d-(17alpha)-13-ethyl-17Âhydroxy-18,19-dinorpregn-4-ene-20-yne-3-one-oxime (further on norelgestromine) via acetylation of d-norgestrel at position 17, oximation of the oxo group at position 3 of the obtained 17-acetoxy derivative, and finally hydrolyzing the acetoxy group at position 17 of the obtained 3-oxime derivative. The process according to our invention is as follows: the starting material, d-(17alpha-17-hydroxy-13-ethyl-18,19-dinorpregn-4-ene-20-yne-3Âone (d-norgestrel) - purity 93-94 % - is acetylated with acetic anhydride in acetic acid, in the presence of zinc chloride and hydrogen chloride, or 70 % perchloric acid in an inert gas atmosphere, and after completion of the reaction the excess of acetic anhydride and the 'enol acetate' by-product are decomposed with aqueous hydrochioric acid, then the formed d-(17alpha)-17-acetoxy-13-ethyl-18,19-dinorpregn-4-ene-20-yne-3-one is isolated from the reaction mixture by addition of ice-water, the precipitated product is filtered off, washed with water, dried, dissolved in dichloromethane or acetone and clarified with silica gel or aluminum oxide and charcoal, after filtration of the clarifier the resulted solution is concentrated and the residue is recrystallized, the obtained d-(17alpha)-17-acetoxy-13-ethyl-18,19-dinorpregn-4-ene-20-yne-3-one is reacted either with hydroxylammonium acetate or with hydroxylammonium chloride in the presence of sodium acetate, in acetic acid in nitrogen atmosphere under vigorous stirring for about 1 hour, after completion of the reaction water is added, the precipitated product is filtered off, washed with water, dried and recrystallized, the obtained d-(17alpha-17-acetoxy-13-ethyl-18,19-dinorpregn-4-ene-20-yne-3-one-oxime is hydrolyzed with an equivalent amount of an alkali metal hydroxide in a C1-C4 alkanol solution, in nitrogen atmosphere between a temperature of about 5-38 °C, under vigorous stirring, after completion of the reaction the mixture is diluted with water and the pH of the resulted suspension is adjusted to 7,5-9 with acetic acid, the precipitated product is filtered off, washed with water, dried, the crude product is dissolved in ethanol, clarified with charcoal, and after filtration of the clarifier water is added to the obtained solution, the precipitated high purity d-(17alpha)-17-acetoxy-13-ethyl-18,19-dinorpregn-4-ene-20-yne-3-one-oxime is filtered off, washed with water and in given case recrystallized from ethanol.
专利号:US-6258960-B1 优先权日:2000-03-17 标题:Catalytic asymmetric synthesis of chiral aziridines 发明人:ANTILLA JON; WULFF WILLIAM D 权利人:ARCH DEV CORP 摘要:The present invention relates to the synthesis of chiral cis-aziridines (IIIa and IIIb) by reacting an imine (I) with a diazo compound (II) in the presence of a chiral vaulted biary-Lewis Acid complex as shown below:
专利号:WO-0056708-A1 优先权日:1999-03-19 标题 :Catalytic asymmetric synthesis of chiral aziridines 发明人:WULFF WILLIAM D; ANTILLA JON 权利人:ARCH DEV CORP 摘要:The present invention relates to the synthesis of chiral cis-aziridines (IIIa and IIIb) by reacting an imine (I) with a diazo compound (II) in the presence of a chiral vaulted biaryl-Lewis Acid complex as shown.
专利号:US-4035425-A 优先权日:1973-04-23 标 题 :Synthesis of Vitamin A, intermediates and conversion thereof to Vitamin A 发明人:OROSHNIK WILLIAM 权利人:SCM CORP 摘要:A synthesis of novel Vitamin A intermediates from beta-ionone is described as well as a conversion of the intermediates to Vitamin A. The length of the conjugated aliphatic side chain of beta-ionone is increased while still ultimately obtaining the desired trans form of Vitamin A. In general, beta-ionone is ethynylated to ethynyl-beta-ionol, the hydroxyl of which is etherified to form an ethynyl-terminated, alkoxy-substituted, beta-ionol intermediate. The intermediate is coupled through its copper derivative with a compound like chloro-isopentenyl acetate to produce a C20 skeleton. By semi-hydrogenation, the acetylenic bond on the C20 skeleton is converted to an ethylenic bond, and by hydrolysis the terminal ester moiety is converted to a hydroxyl group. Treatment with a strong base removes the alkoxy group to produce Vitamin A.
专利号:US-4092366-A 优先权日:1975-04-10 标题:Synthesis of Vitamin A, intermediates and conversion thereof to Vitamin A 发明人:OROSHNIK WILLIAM 权利人:SCM CORP 摘要:A synthesis of novel Vitamin A intermediates from betaionone is described as well as a conversion of the intermediates to Vitamin A. The length of the conjugated aliphatic side chain of beta-ionone is increased while still ultimately obtaining the desired trans form of Vitamin A. In general, beta-ionone is ethynylated to ethynyl-beta-ionol, the hydroxyl of which is etherified to form an ethynyl-terminated, alkoxy-substituted, beta-ionol intermediate. The intermediate is coupled through its copper derivative with a compound like chloro-isopentenyl acetate to produce a C20 skeleton. By semi-hydrogenation, the acetylenic bond on the C20 skeleton is converted to an ethylenic bond, and by hydrolysis the terminal ester moiety is converted to a hydroxyl group. Treatment with a strong base removes the alkoxy group to produce Vitamin A.
参考文献:10.1021/pr200310s 摘要:Manna SK, Patterson AD, Yang Q, Krausz KW, Idle JR, Fornace AJ, Gonzalez FJ. UPLC-MS-based urine metabolomics reveals indole-3-lactic acid and phenyllactic acid as conserved biomarkers for alcohol-induced liver disease in the Ppara-null mouse model. J Proteome Res. 2011 Sep 02;10(9):4120–33. 参考文献:10.1021/jp204557d 摘要:Szafrański M. Crystal Structures, Phase Transitions, and Pressure-Induced Ferroelectricity in [C(NH2)3]5SO4(SO3–OC2H5)2F. J. Phys. Chem. B. 2011 Aug 10;115(34):10277–84. doi: 10.1021/jp204557d.