专利号:US-5521310-A 优先权日:1992-10-07 标 题 :Process to obtain benzoxazines to be used for the synthesis of ofloxazine, levofloxazine and derivatives 发明人:CARRETERO GONZALVEZ JUAN-CARLO; VICIOSO SANCHEZ MERCEDES; GARCIA RUANO JOSE-LUIS 权利人:ETILO DERIVADOS 摘要:A process to obtain benzoxazines useful for the synthesis of Ofloxazine, Levofloxazine and derivatives. The benzoxacines (I) where Xb is an halogen and R 1 is H, alkyl or alkenyl of up to 6 atoms of C or aryl, can be obtained by means of cycling a compound of formula (II) through the reaction with triphenylphosphine and ethyl azodicarboxilate. The compounds of formula (II) can be obtained through the reaction of a compound (III) with an adequate epoxide. Through the use of the adequate chiral epoxide it is possible to obtain the enantiomerically desired intermediate and, therefore and selectively, it is possible to obtain the desired final product with the adequate enantiomeric form without the need to carry out a resolution stage. n The Compounds (I) are useful and key intermediates for the synthesis of the antimicrobials Oflixazine and Levofloxazine. ##STR1##
专利号:US-7038062-B2 优先权日:2004-07-01 标题:Synthesis of cyclic trithiocarbonates from epoxides 发明人:PARKER DANE KENTON 权利人:GOODYEAR TIRE & RUBBER 摘要:This invention provides a low cost technique for synthesizing cyclic trithiocarbonates by a simple one step process from epoxides that can be conducted under atmospheric pressure. This synthesis can be depicted as follows: n nwherein R represents a moiety selected from the group consisting of alkyl groups and aryl groups, wherein R′ represents a moiety selected from the group consisting of alkyl groups, aryl groups, and hydrogen atoms, and wherein R″ represents a moiety selected from the group consisting of alkyl groups, aryl groups, and hydrogen atoms, wherein the R moiety and the R′ moiety can be bonded together to form a cyclic structure, with the proviso that R″ represents a hydrogen atom if R′ represents an alkyl group or an aryl group. In this process carbon disulfide and a thiocyanate salt, such as potassium thiocyanate, are reacted with the epoxide in an ionic liquid, such as 1-butyl-3-methylimidazolium hexafluorophosphate ([Bmim] PF 6 ) in the presence of water to produce the cyclic trithiocarbonate.
专利号:US-2018111938-A1 优先权日:2015-05-05 标 题:Synthesis of Intermediates Used in the Manufacture of Anti-HIV Agents 发明人:PRADHAN BRAJA SUNDAR; AMARNATH KOMMIREDDY; VEMPALA NARESH; RAHMAN MD ATAUR 权利人:CBZ INVEST LTD 摘要:The present invention relates to a process of preparing intermediates of Formula (I). The process comprises of reacting compound of Formula (III) with compound of Formula (V) in the presence of a solvent selected from an alcohol, ether or water to form compound of Formula (I) wherein, R 1 is selected from —NH 2 , Cl, Br, NHCOR″, wherein R″ is alkyl, aryl, Schiff's base of formula Nâ•?CHR′, wherein R′ is alkyl or aryl; R 2 is selected from H, alkyl; R 3 and R 4 , each independently is H; R 5 and R 6 , each independently is H, alkyl; R 7 is H, alkyl; and R 8 is H, alkyl.
专利号:US-10266503-B1 优先权日:2016-05-24 标 题 :Sulfoxide ligand metal catalyzed oxidation of olefins 发明人:WHITE M CHRISTINA; AMMANN STEPHEN E; LIU WEI; MA RULIN 权利人:UNIV ILLINOIS 摘要:The enantioselective synthesis of isochroman motifs has been accomplished via Pd(II)-catalyzed allylic C—H oxidation from terminal olefin precursors. Critical to the success of this goal was the development and utilization of a novel chiral aryl sulfoxide-oxazoline (ArSOX) ligand. The allylic C—H oxidation reaction proceeds with the broadest scope and highest levels asymmetric induction reported to date (avg. 92% ee, 13 examples ≥90% ee). Additionally, C(sp 3 )-N fragment coupling reaction between abundant terminal olefins and N-triflyl protected aliphatic and aromatic amines via Pd(II)/sulfoxide (SOX) catalyzed intermolecular allylic C—H amination is disclosed. A range of 52 allylic amines are furnished in good yields (avg. 76%) and excellent regio- and stereoselectivity (avg. >20:1 linear:branched, >20:1 E:Z). For the first time, a variety of singly activated aromatic and aliphatic nitrogen nucleophiles, including ones with stereochemical elements, can be used in fragment coupling stiochiometries for intermolecular C—H amination reactions.
专利号:US-6720439-B1 优先权日:2001-09-28 标题:Synthesis of ruthenium-hydride complexes and preparation procedures of chiral alcohols and ketones 发明人:OHKUMA TAKESHI; KOIZUMI MASATOSHI; MUNIZ KILIAN; NOYORI RYOJI 权利人:INST NAGOYA IND SCIENCE RES 摘要:trans-RuH(eta<1>-BH4)[(S)-xylbinap][(S,S)-dpen] (0.00125 mmol), acetophenone (5.0 mmol), and 2-propanol (2.5 mL) were placed in an autoclave, and the resulting solution was repeatedly subject 5 times to a procedure of performing pressure reduction and argon introduction while stirring the solution for deaeration. A hydrogen tank was then connected to the autoclave, and after replacing the air inside an introduction tube with hydrogen, the pressure inside the autoclave was adjusted to 5 atmospheres and then hydrogen was released until the pressure dropped to 1 atmosphere. After repeating this procedure 10 times, the hydrogen pressure was adjusted to 8 atmospheres and stirring at 25° C. was performed for 12 hours. By concentrating the solution obtained by depressurization and subjecting the crude product to simple distillation, (R)-1-phenylethanol (yield: 95%) in the form of a colorless oily substance was obtained at an ee of 99%.
专利号:US-6448449-B2 优先权日:2000-04-21 标题:Process for preparation of (R)-1- (aryloxy)propan-2-ol 发明人:LARROW JAY FRANCIS 权利人:RHODIA CHIREX INC 摘要:A process for the preparation of (R)-1-(2,3-difluoro-6-nitrophenoxy)-propan-2-ol, which is a useful intermediate in the synthesis of the widely used antibiotic Levofloxacin is provided. A process for the preparation of (R)-1-(2,3-difluoro-6-nitrophenoxy)-2-trimethylsiloxypropane is also described. The process includes the ring opening of (R)-propylene oxide with 2,3-difluoro-6-nitrophenyl trimethylsilyl ether in the presence of an optically active Co(salen) catalyst. The trimethylsilyl group of the reactant is transferred to the product aryloxy alcohol, which serves to protect the secondary alcohol in situ. Upon isolation, the trimethylsilyl group is removed and the resulting regioisomeric mixture purified to yield the desired (R)-1-(2,3-difluoro-6-nitrophenoxy)-propan-2-ol in high purity and yield.
参考标题:Synthesis Of Spiroacetal Pheromones Via Metalated Hydrazones 作者:Dieter Enders,Walter Dahmen,Eleonore Dederichs,Winfried Gatzweiler,Peter Weuster 摘要:The Synthesis Of Simple Alkyl Substituted Spiroacetals By î+/-,î+/-′-Alkylation Of Metalated Acetone Dimethylhydrazone With Appropriate Electrophiles And Subsequent Acid Catalyzed Cleavage And Ring Closure Of The Products Is Described.
合成参考文献
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