(Azido(Ethylperoxy)Methyl)Benzene置于1,8-二氮杂双环[5.4.0]十一碳-7-烯体系中,用 乙酸乙酯 作为反应溶剂,化学反应 3.0H,以90 Mg的收率获得产物苯甲酸乙酯 参考文献:Intramolecular Rearrangement Of α-Azidoperoxides: An Efficient Synthesis Of Tert-Butyl Esters 标题:Intramolecular Rearrangement Of α-Azidoperoxides: An Efficient Synthesis Of Tert-Butyl Esters 摘要:An Unprecedented Intramolecular Rearrangement Of Alpha-Azidoperoxides,Promoted By Simple Organic Base To Provide Tert-Butyl Esters,Has Been Presented. Further,A One-Pot Methodology Consisting Of In Situ Generation Of The A-Azidoperoxides From Corresponding Aldehydes Followed By Base-Promoted Rearrangement To Obtain The Desired Ester Has Also Been Executed. Relevant Mechanistic Studies,To Provide The Proof For Intramolecular Alkoxy Transfer,Are Investigated. DOI:10.1021/acs.Orglett.5B00190
专利号:US-3836544-A 优先权日:1972-04-25 标 题:Synthesis of zearalanes ii and related compounds and intermediates useful in the syntheses thereof 发明人:URRY W; MULLENBACH G 权利人:COMMERCIAL SOLVENTS CORP 摘要:THIS INVENTION PROVIDES A NEW SYNTHESIS FOR NORZEARALANE II AND RELATED COMPOUNDS WHICH RELATED COMPOUNDS AND NORZEARALANE II ARE REPRESENTED BY THE FORMULA 1,5-DI(HO-),2,3-(-CO-O-CH2-(CH2)X-)-BENZENE WHERE X IS AN INTEGER HAVING A VALUE FROM 1 TO 13 INCLUSIVE. THE ANABOLIC AGENT NORZEARALANE II, IN WHICH X=9 IN THEFOREGOING FORMULA, IS PREPARED BY A TOTAL CHEMICAL SYNTHESIS INVOLVING THE REACTION OF 10-UNDECENAL WITH MALONIC ACID TO PRODUCE TRANS-2,12-TRIDECADIENOIC ACID; TREATING THE ACID SO FORMED WITH DIAZOMSTHANE TO YIELD METHYL TRANS-2,12-TRIDECADIENOATE; REACTING THE METHYL ESTER WITH ETHYL ACETOACETATE AND SODIUM ETHOXIDE TO FORM THE SODIUM SALT OF ETHYL 6-(9-DECENYL)-B-DIHYDRORESORCYLATE; BROMINATING THE DIHYDRORESORCYLATE TO PREPARE ETHYL 3-BROMO- 6 - (9-DECENYL)-B-DIHYDRORESOCRYLATE; DE-HYDROBROMINATING THE FOREGOING BROMO DERIVATIVE TO GIVE ETHYL 6-(9-DECENYL)-B-RESORCYLATE; REACTING THE RESORCYLATE ESTER WITH BENZYL CHLORIDE TO PRODUCE ETHYL 6-(9-DECENYL)-BRESORCYLATE DIBENZYL ETHER; SUBJECTING THE BENZYLATED ESTER TO THE ACTION OF DIBORANE, WATER AND HYDROGEN PEROXIDE TO FORM ETHYL 2,4-BIS (BENZYLOXY)-6-(10-HYDROXYDECYL)BENZOATE; TREATING THE FOREGOING BENZOATE WITH SODIUM ETHOXIDE TO PREPARE NORZEARALANE II DIBENZYL ETHER, ONE ALSO TO PREPARE AS A BY-PRODUCT THE DIMERIC DILACTONE OF 2,4-BIS(BENZYLOXY)-6-(10-HYDROXYDECYL)-BENZOIC ACID; HYDROGENATING NORZEARALANE II DIBENZYL ETHER TO FORM NORZEARALANE II. IN GENERAL, A HOMOLOGUE OF NORZEARALANE II AND/OR OF THE CORRESPONDING DIMERIC DILACTONE IS PREPARED BY SUBSTITUTING FOOR 10-UNDECENAL IN THE FOREGOING SEQUENCE OF REACTIONS AN UNSATURATED ALDEHYDE HAVING THE FORMULA CH2=CH-(CH2)X-1-CHO WHERE X IS AN INTEGER WHICH MAY HAVE THE VALUE 1,2,3,4, 5, 6, 7, 8, 9, 10, 11, 12 OR 13 SPECIFICALLY ZEARALANE II (WHERE X=10) IS PREPARED STARTING WITH 11-DODECENAL AND THE DIMERIC DILACTONE FROM 6-(5-HYDROXYPENTYL-B-RESORCYCLIC ACID DIBENZYL ETHER IS PREPARED WHEN THE STARTING ALDEHYDE IS 5-HEXENAL (WHERE X= 4) THE INVENTION ALSO COVERS PHYSIOLOGICALLY ACTIVE COMPOUNDS RELATED TO THE ZEARALANES II AND KNOW AS DIMERIC DILACTONES HAVING THE FORMULA, 1,5-DI(RO-),2,3-(-CO-O-CH2-(CH2)X-(3,5-DI(RO-)-1,6-PHENYL ENE)-CO-O-CH2-(CH2)X-)-BENZENE X IS AN INTEGER WHICH MAY HAVE THE VALUE 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12 OR 13 AND WHERE R IS EITHE HYDROGEN OR A BENZYL RADICAL (C6H5CH2-). MORE PARTICULARLY, THIS INVENTION RELATES TO NOVEL INTERMEDIATES PRODUCED IN THE SYNTHESIS OF THE ABOVE COMPOUNDS AND TO PROCESSES FOR MAKING THESE INTERMEDIATES.
专利号:US-8058414-B2 优先权日:2008-04-29 标题 :Unnatural polymerase substrates that can sustain enzymatic synthesis of double stranded nucleic acids from a nucleic acid template and methods of use 发明人:MENCHEN STEVEN; ROSENBLUM BARNETT; KENNEY PAUL; KHAN SHOEB; MA ZHAOCHUN; CHEN JER-KANG; LAM JOE Y; HUANG BOLI 权利人:MENCHEN STEVEN; ROSENBLUM BARNETT; KENNEY PAUL; KHAN SHOEB; MA ZHAOCHUN; CHEN JER-KANG; LAM JOE Y; HUANG BOLI; LIFE TECHNOLOGIES CORP 摘要:Nucleotide analogs that can sustain the enzymatic synthesis of double-stranded nucleic acid from a nucleic template are described. The nucleotide analogs include: (i) a base selected from the group consisting of adenine, guanine, cytosine, thymine, uracil and their analogs; (ii) a label attached to the base or analog of the base via a cleavable linker; (iii) a deoxyribose; and (iv) one or more phosphate groups. The linker and/or the label inhibits template directed polymerase incorporation of a further nucleotide substrate onto an extended primer strand. In addition, cleavage of the linker leaves a residue attached to the base which is not present in the natural nucleotide and which does not inhibit extension of the primer strand. The nucleotide analogs can therefore be used as reversible terminators in sequencing by synthesis methods without blocking the 3′ hydroxyl group. Methods of sequencing DNA using the substrates are also described.
专利号:US-2007260076-A1 优先权日:2003-12-05 标 题:Practical, Cost-Effective Synthesis of Ubiquinones 发明人:LIPSHUTZ BRUCE H; BERL VOLKER; SHEIN KARIN; WETTERICH FRANK 权利人:LIPSHUTZ BRUCE H; BERL VOLKER; SHEIN KARIN; WETTERICH FRANK 摘要:The present invention provides a convergent method for the synthesis of ubiquinones and ubiquinone analogues. Also provided are precursors of ubiquinones and their analogues that are useful in the methods of the invention. The invention further provides an improved method for the carboalumination of alkyne substrates.
专利号:US-2006167289-A1 优先权日:2003-12-05 标题 :Practical, cost-effective synthesis of ubiquinones 发明人:LIPSHUTZ BRUCE H; BERL VOLKER; SCHEIN KARIN; WETTERICH FRANK 权利人:ZYMES LLC 摘要:The present invention provides a convergent method for the synthesis of ubiquinones and ubiquinone analogues. Also provided are precursors of ubiquinones and their analogues that are useful in the methods of the invention. The invention further provides an improved method for the carboalumination of alkyne substrates.
专利号:US-8283424-B2 优先权日:2008-03-18 标题 :Process for the synthesis of alpha-olefin polymerization procatalysts 发明人:GUPTA VIRENDRAKUMAR; PATIL HARSHAD RAMDAS; NAIK DHANANJAY GHELABHAI 权利人:GUPTA VIRENDRAKUMAR; PATIL HARSHAD RAMDAS; NAIK DHANANJAY GHELABHAI; RELIANCE IND LTD 摘要:The invention relates to a process for the synthesis of a Ziegler Natta procatalyst, the process comprising first treating magnesium alkoxide with a twice used mixed solvent of TiCl 4 and chlorobenzene to form a first stage product, then treating the first stage product with a once used mixed solvent of TiCl 4 and chlorobenzene to form a second stage product and finally treating the second stage product with mixed solvent recovered by treatment of effluent from the first treatment with benzoyl chloride so as to convert contaminant of formula TiCl 3 OR in the effluent to an addition complex which is precipitated, filtered off and hydrolyzed to recover ethyl benzoate and to form Ti(OH) 4 as a side product, the product after final treatment being subjected to a plurality of successive washing steps with used as well as recovered hexane.
专利号:US-5166110-A 优先权日:1989-12-22 标 题 :Process for the synthesis of ziegler-type catalytic solids or solid constituents of the same 发明人:BRUN CLAUDE 权利人:ATOCHEM ELF SA 摘要:A process is provided for the synthesis of a solid Ziegler catalyst or of a transition metal solid constituent thereof, which entails preparing the solid catalyst or constituent thereof as a suspension in an inert liquid medium by contacting precursors or ingredients of the catalyst or of the constituent in the inert liquid medium in one or more steps, and drying the suspension, and collecting the catalyst or constituent thereof; and wherein the process is conducted in a single multi-function reactor having a longitudinal axis and which can pivot around an axis which intersects perpendicularly with this axis.
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合成参考文献
摘要:Schobert, R.; Hölzel, C.; Barnickel, B., Science of Synthesis, (2010) 47, 50. 摘要:Kaminsky, W., Science of Synthesis, (2009) 48, 718. 摘要:Petasis, N. A., Science of Synthesis, (2010) 47, 232. 摘要:Petasis, N. A., Science of Synthesis, (2010) 47, 214. 摘要:Weibel, J.-M.; Blanc, A.; Pale, P., Science of Synthesis Knowledge Updates, (2018) 1, 42.