专利号:US-8129521-B2 优先权日:2005-12-14 标 题 :One pot synthesis of tetrazole derivatives of rapamycin 发明人:DHAON MADHUP K; HSIAO CHI-NUNG; PATEL SUBHASH R; BONK PETER J; CHEMBURKAR SANJAY R; CHEN YONG Y 权利人:DHAON MADHUP K; HSIAO CHI-NUNG; PATEL SUBHASH R; BONK PETER J; CHEMBURKAR SANJAY R; CHEN YONG Y; ABBOTT LAB 摘要:A single-step, one-pot process to obtain zotarolimus and other rapamycin derivatives on large scale is presented, which improves currently available synthesis schemes. In one embodiment, dried rapamycin is dissolved in isopropylacetate (IPAc). The solution is cooled, and 2,6-Lutidine is added, followed slowly adding triflic anhydride at −30° C. Salts are then removed by filtration. Tetrazole, followed by a tert-base diisopropylethylamine (DIEA) is added to the triflate solution. After incubation at room temperature, the product is concentrated and purified by a silica gel column using THF/heptane as eluant. The fractions containing the product are collected, concentrated, and purified again using an acetone/heptane column. The product containing fractions are concentrated. The product is dissolved in t-BME and precipitated with heptane. The solids are dissolved in acetone, treated with butylated-hydroxy toluene (BHT), and the solution concentrated. The process is repeated twice with acetone to remove solvents. At least one stabilizing agent is added, such as BHT at 0.5% before drying.
专利号:US-2009318592-A1 优先权日:2005-10-11 标 题 :Process for the Synthesis of Amine Ethers 发明人:FREY MARKUS; BROENNIMANN VALERIE 权利人:CIBA GEIGY CORP 摘要:The present invention relates to novel processes for the preparation of a sterically hindered amine ether by reacting a corresponding sterically hindered amine oxide with a ketone or an aldehyde with at least one reactive H in the presence of a peroxydisulphate. Products obtained by this process may be hydrogenated. The compounds made by these processes are particularly effective in the stabilization of polymer compositions against harmful effects of light, oxygen and/or heat and as flame-retardants for polymers.
专利号:US-2007191516-A1 优先权日:2004-03-15 标题 :Process for the synthesis of amine ethers 发明人:FREY MARKUS; RAST VALERIE; BRAIG ADALBERT; KRAMER ANDREAS 权利人:FREY MARKUS; RAST VALERIE; BRAIG ADALBERT; KRAMER ANDREAS 摘要:A process for the preparation of a sterically hindered amine ether which comprises reacting a corresponding sterically hindered aminoxide with a C 5 -C 18 alk-1-ene in the presence of an organic hydroperoxide and optionally hydrogenating the resulting product as well as the product mixtures obtained therewith and their use as stabilizers and flame retardants.
专利号:US-2004110228-A1 优先权日:2002-04-01 标 题:Combinatorial organic synthesis of unique biologically active compounds 发明人:MCALPINE SHELLI R; TAYLOR RACHEL E; BOLLA MEGAN L; SEGALL ANCA M 摘要:The invention provides a method for making a combinatorial library of cyclic compounds, such as Holliday junction-trapping compounds, comprising the steps of (a) obtaining a plurality of trimers according to the generic structure X 1- X 2- X 3 , wherein X 1 , X 2 and X 3 can be independently any naturally or nonnaturally occurring amino acids or peptidomimetics thereof; (b) optionally coupling a spacer S to the trimer at either end; (c) cyclizing two trimers or trimer-spacer conjugates in a head-to-tail orientation; thereby obtaining a combinatorial library of compounds, wherein the library does not include an unmodifed or naturally occurring Holliday Junction-trapping compounds. The invention additionally provides methods macrocyclic compounds that are synergimycin derivatives.
专利号:US-3631185-A 优先权日:1970-04-10 标题 :Synthesis of 2 4 6-tri-t-butyl-4-methoxycyclohexa-2 5-dien-1-one 发明人:LAUFER ROBERT J 权利人:CONSOLIDATION COAL CO 摘要:THE COMPOUND 2,4,6-TRI-T-BUTYL-4-METHOXYCYCLOHEXA2,5-DIEN-1-ONE, HAVING THE FOLLOWING STRUCTURAL FORMULA 1,3,5-TRI(T-C4H9-),5-(CH3-O-)CYCLOHEXA-2,5-DIEN-1-ONE IS SYNTHESIZED IN ONE STEP BY REACTING 2,4,6-TRI-T-BUTYLPHENOL, BROMINE, METHANOL AND AN ALKALI METAL CARBONATE AT A TEMPERATURE WITHIN THE RANGE 20 TO 80*C. THE PRODUCT COMPOUND HAVING THE ABOVE FORMULA IS PRODUCED IN 65 PERCENT OR BETTER YIELD. IT IS USEFUL AS AN INTERMEDIATE IN THE PREPARATION OF 2,6-DI-T-BUTYL-4-METHOXYPHENOL OR 2-T-BUTYL-4-METHOXYPHENOL, BOTH OF WHICH ARE USEFUL AS ANTIOXIDANTS, THE FORMER IN NON-FOOD USES AND THE LATTER IN FOODS.
专利号:US-7402675-B2 优先权日:2000-05-26 标题 :Process for the synthesis of amine ethers from secondary amino oxides 发明人:HAFNER ANDREAS; KIRNER HANS JUERG; SCHWARZENBACH FRANZ; VAN DER SCHAAF PAUL ADRIAAN; NESVADBA PETER 权利人:CIBA SC HOLDING AG 摘要:An amine ether of formula A n nwherein a is 1 or 2; and when a is 1, E is E′; when a is 2, E is L;n E′ is C 1 -C 36 alkyl; C 3 -C 18 alkenyl; C 2 -C 18 alkinyl; C 5 -C 18 cycloalkyl; C 5 -C 18 cycloalkenyl; a radical of a saturated or unsaturated aliphatic bicyclic or tricyclic hydrocarbon of 7 to 12 carbon atoms; C 2 -C 7 alkyl or C 3 -C 7 alkenyl substituted by halogen; C 7 -C 15 aralkyl or C 7 -C 15 aralkyl substituted by C 1 -C 4 alkyl or phenyl; or E′ is a radical of formula (VII) as explained in claim 1; T′ is tertiary C 4 -C 18 alkyl or phenyl, each of which are unsubstituted or substituted by halogen, OH, COOR 21 or C(O)—R 22 ; or T′ is C 5 -C 12 cycloalkyl; C 5 -C 12 cycloalkyl which is interrupted by at least one O or —NR 18 —; a polycyclic alkyl radical having 7-18 carbon atoms, or the same radical which is interrupted by at least one O or —NR 18 —; or T′ is —C(G 1 )(G 2 )-T″; or C 1 -C 18 alkyl or C 5 -C 12 cycloalkyl substituted by n n n n n n n n n n n n T″ is hydrogen, halogen, NO 2 , cyano, or is a monovalent organic radical comprising 1-50 carbon atoms; n or T″ and T′ together form a divalent organic linking group completing, together with the hindered amine nitrogen atom and the quaternary carbon atom substituted by G 1 and G 2 , an optionally substituted five- or six-membered ring structure; and all other residues are as defined in claim 1, n are obtained in good yield from the corresponding N-oxyl hindered amine precursor by reaction with a hydrocarbon E 1 -H or H-L-H in the presence of an organic hydroperoxide and a catalytic amount of copper or a copper compound. n n n n n The products of present process find utility as polymerization regulators and/or light stabilizers for organic material.
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合成参考文献
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