1,2-二氯乙烷置于calcium Iodide体系中,化学反应生成 1,2-二碘乙烷 参考文献:Spindler,Justus Liebigs Annalen Der Chemie,1885,Vol. 231,P. 272 标题:Spindler,Justus Liebigs Annalen Der Chemie,1885,Vol. 231,P. 272
专利信息
专利号:US-10011580-B2 优先权日:2016-04-21 标题:Diastereoselective synthesis of (±)-epianastrephin, (±)-anastrephin and analogs thereof 发明人:WALSE SPENCER S; KUZMICH DANIEL 权利人:US AGRICULTURE 摘要:A process for the synthesis of trans-fused γ-lactones having Formula (IV) from substituted cyclic ketones having Formula (I). A diastereoselective synthesis of (±)-epianastrephin (1) (wherein: R 1 is ethenyl, R 2 and R 3 is methyl, and n is 1), (±)-anastrephin (2) (wherein: R 2 is ethenyl, R 1 and R 3 is methyl and n is 1), and analogs thereof (wherein: R 1 is H, C 1-5 alkyl, C 2-6 alkenyl or C 2-6 alkynyl, R 2 is H, C 1-5 alkyl, C 2-6 alkenyl or C 2-6 alkynyl, R 1 and R 2 together with the carbon atom they are attached form a C 3-6 cycloalkyl ring, R 3 is C 1-5 alkyl and n is 0-2):
专利号:WO-2012003598-A1 优先权日:2010-07-06 标 题 :Intermediates for the synthesis of 1,2-bis(4,7-dimethyl-1,4,7-triazacyclonon-1-yl)-ethane and preparation method thereof 发明人:HAGE RONALD; KOEK JEAN HYPOLITES; RUSSELL STEPHEN WILLIAM; WANG XIAOHONG; WOLF LODEWIJK VAN DER; ZHANG JIANRONG; ZHAO WEI 权利人:UNILEVER PLC; UNILEVER NV; UNILEVER HINDUSTAN; HAGE RONALD; KOEK JEAN HYPOLITES; RUSSELL STEPHEN WILLIAM; WANG XIAOHONG; WOLF LODEWIJK VAN DER; ZHANG JIANRONG; ZHAO WEI 摘要:The present invention provides intermediates for the synthesis of 1,2-bis(4,7-dimethyl-1,4,7-triazacyclonon-1-yl)-ethane and preparation method thereof. The intermediates are protonated salts of 1,4-ditosylate-1,4,7-triazacyclononane or 1,4-dibenzenesulphonate-1,4,7-triazacyclononane. The preparation method of 1,4-diarylsulfonate-1,4,7-triazacyclononane (compound A) comprises reacting 1,4,7-triarylsulfonate-1,4,7-triazacyclononane (compound B) in an acidic medium comprising sulphuric acid, wherein the molar ratio of B to sulphuric acid is in the range from 1 : 0.5 to 1 : 10, or reacting 1,4,7-triarylsulfonate-1,4,7-triazacyclononane (compound B) in an acidic medium and working up the acidic medium when the conversion of B to A is at least 50 mol % yielding compound A.
专利号:US-8907082-B2 优先权日:2010-07-06 标 题 :1,2-bis-(4,7-dimethyl-1,4,7-triazacyclonon-1-yl)-ethane and intermediate for the synthesis of same 发明人:HAGE RONALD; KOEK JEAN HYPOLITES; RUSSELL STEPHEN WILLIAM; VAN DER WOLF LODEWIJK; ZHANG JIANRONG; ZHAO WEI; WANG XIAOHONG 权利人:HAGE RONALD; KOEK JEAN HYPOLITES; RUSSELL STEPHEN WILLIAM; VAN DER WOLF LODEWIJK; ZHANG JIANRONG; ZHAO WEI; WANG XIAOHONG; CATEXEL LTD 摘要:The present invention provides improved processes for the synthesis of 1,4-ditosyl-1,4,7-triazacyclonone, comprising deprotecting a compound of formula (C): n nwherein P is tosylate or arylsulfonate, with an acidic medium to form 1,2-bis(1,4,7-triazacyclonon-1-yl)-ethane; and subsequently adding formaldehyde and formic acid to the acidic medium to form 1,2-bis-(4,7-dimethyl-1,4,7-triazacyclonon-1-yl)-ethane (Me 4 -DTNE). The syntheses of intermediates are also disclosed.
专利号:US-7078572-B2 优先权日:2002-09-20 标题:Process for the synthesis of intermediates useful for the synthesis of tubulin inhibitors 发明人:KENDALL JOHN THOMAS 权利人:WYETH CORP 摘要:The invention is a process for the preparation of compounds of the Formula I: n nwhere R 1 , R 2 , R 3 , R 4 and R 5 are defined in the specification, which are intermediates useful for the preparation of tubulin inhibitors which are useful in the treatment of cancer.
专利号:US-2007042987-A1 优先权日:2004-07-30 标题:Stereoselective synthesis of beta-nucleosides 发明人:LIN KO-CHUNG; LI WENSEN; LIN CHUNHUI; YUNGSHUN WEIN; KUO-HIS KAO 权利人:LIN KO-CHUNG; LI WENSEN; LIN CHUNHUI; YUNGSHUN WEIN; KUO-HIS KAO 摘要:This invention relates to a process of stereoselectively synthesizing an alcohol of the following formula: n n nwherein R 1 , R 2 , R 3 , R 4 , and R 5 are defined in the specification. The process includes reacting (R) 4-formyl-2,2-dimethyldioxolane with α-bromoacetate in the presence of Zn and a Zn activating agent.
专利号:US-7485716-B2 优先权日:2005-05-02 标题:Stereoselective synthesis of β-nucleosides 发明人:LIN KO-CHUNG; LI WENSEN 权利人:PHARMAESSENTIA CORP 摘要:This invention relates to a process for stereoselectively preparing a nucleoside of the following formula: n nwherein R 3 , R 4 , and B are defined herein. The process includes reacting a furanose compound with a nucleobase in the presence of a halide salt. Also disclosed is another process for stereoselectively synthesizing an intermediate that can be used to make the starting compound in the first-mentioned process.
[参考文献]: André M Bienfait, Et Al. Europium Bis(Dimethylsilyl)Amides Including Mixed-Valent Eu3[n(Sihme2)2]6[μ-N(Sihme2)2]2. Dalton Trans. 2014 Dec 14;43(46):17324-32.
合成参考文献
摘要:Chciuk, T. V.; Flowers, R. A.; Flowers, R. A., Science of Synthesis Knowledge Updates, (2016) 2, 178. 摘要:Chciuk, T. V.; Flowers, R. A.; Flowers, R. A., Science of Synthesis Knowledge Updates, (2016) 2, 183. 摘要:Chciuk, T. V.; Flowers, R. A.; Flowers, R. A., Science of Synthesis Knowledge Updates, (2016) 2, 181. 摘要:Chciuk, T. V.; Flowers, R. A.; Flowers, R. A., Science of Synthesis Knowledge Updates, (2016) 2, 181. 摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2010) 2, 350.