三苯基膦置于氢溴酸体系中,化学反应 0.08H,以97%的收率获得产物三苯基膦氢溴酸盐 参考文献:Triphenylphosphonium Bromide: A Convenient And Quantitative Source Of Gaseous Hydrogen Bromide 标题:Triphenylphosphonium Bromide: A Convenient And Quantitative Source Of Gaseous Hydrogen Bromide 摘要:在回流二甲苯中对三苯基溴化膦进行热解,可得到定量的无水溴化氢. DOI:10.1055/s-1988-27502
专利号:US-7939679-B2 优先权日:2006-01-19 标题:Method for synthesis of ciguatoxin CTX1B and compounds useful for the synthesis of ciguatoxin CTX1B 发明人:HIRAMA MASAHIRO; INOUE MASAYUKI 权利人:JAPAN SCIENCE & TECH AGENCY 摘要:Disclosed is a method for total synthesis of CTX1B, which is developed for the synthesis of a ciguatoxin analogue such as CTX3C and enables the more efficient application of an established reaction to the total synthesis of CTC1B. More specifically, disclosed is a method for total synthesis of CTX1B comprising; an O.S-acetal formation for synthesizing a novel compound (3); a radical cyclization reaction for constructing a 9-membered ring formation reaction including a novel compound (6) through a novel compound (8) and yielding a compound (D); and a deprotection for yielding CTX1B. Also disclosed are novel compounds (1) to (8) which are particularly useful for synthesis of CTX1B and can be used for the synthesis of a ciguatoxin analogue.
专利号:US-8822702-B2 优先权日:2002-12-20 标 题 :Synthesis of amines and intermediates for the synthesis thereof 发明人:BERENS ULRICH; DOSENBACH OLIVER; SPRENGER DANIEL 权利人:BERENS ULRICH; DOSENBACH OLIVER; SPRENGER DANIEL; BASF SE 摘要:The invention relates in a first embodiment to a method for the manufacture of esters of the formula I, n nor especially of amides of the formula II,n n nwherein the symbols have the meanings given in the specification, as well as other intermediates and compounds useful in the synthesis of tryptamines and other substances mentioned in the title. The synthesis methods and intermediates are useful in the synthesis of pharmaceuticals.
专利号:US-3992413-A 优先权日:1975-07-25 标 题 :Intermediates in the synthesis of prostaglandins 发明人:TAUB DAVID; WENDLER NORMAN L 权利人:MERCK & CO INC 摘要:The invention relates to a new and novel synthesis of prostaglandin E 2 , and it particularly relates to a novel process starting with relatively inexpensive starting materials. The invention further relates to a synthesis which is readily adaptable for large scale processing because of the high yields in the individual reaction steps. n The invention further relates to novel compounds formed as intermediates in the synthesis of prostaglandin E 2 . The invention still further relates to synthetic analogs and known metabolites of prostaglandin E 2 and prostaglandin E 1 , useful as standards in certain biological assays for determining prostaglandin-like activity.
专利号:US-8222458-B2 优先权日:2008-06-13 标题 :Process or synthesis of (3S)- and (3R)-3-hydroxy-beta-ionone, and their transformation to zeaxanthin and beta-cryptoxanthin 发明人:KHACHIK FREDERICK; CHANG AN-NI 权利人:KHACHIK FREDERICK; CHANG AN-NI; UNIV MARYLAND 摘要:Disclosed is a process for the synthesis of (3R)-3-hydroxy-β-ionone and its (3S)-enantiomer in high optical purity from commercially available (rac)-α-ionone. The key intermediate for the synthesis of these hydroxyionones is 3-keto-α-ionone ketal that was prepared from (rac)-α-ionone after protection of this ketone as a 1,3-dioxolane. Reduction of 3-keto-α-ionone ketal followed by deprotection, lead to 3-hydroxy-α-ionone that was transformed into (rac)-3-hydrox-β-ionone by base-catalyzed double bond isomerization in 46% overall yield from (rac)-α-ionone. The racemic mixture of these hydroxyionones was then resolved by enzyme-mediated acylation in 96% ee. (3R)-3-Hydroxy-β-ionone and its (3S)-enantiomer were respectively transformed to (3R)-3-hydroxy-(β-ionylideneethyl)triphenylphosphonium chloride [(3R)-C 15 -Wittig salt] and its (3S)-enantiomer [(3S)-C 15 -Wittig salt] according to known procedures. Double Wittig condensation of these Wittig salts with commercial available 2,5- dimethtylocta-2,4,6-triene-1,8-dial provided all 3 stereoisomers of zeaxanthin. Similarly, (3R)-C 15 -Wittig and its (3S)-enantiomer were each coupled with β-apo-12′-carotenal.
专利号:US-9422326-B2 优先权日:2012-09-04 标 题:Process for preparing 11-methylene-18-methyl-estr-4-en-3, 17-dione, useful as intermediate compound for the synthesis of molecules having pharmacological activity 发明人:LENNA ROBERTO; MARIANI EDOARDO; VANOSSI ANDREA 权利人:IND CHIMICA SRL 摘要:There is described a process for the industrial synthesis of 11-methylene-18-methyl-estr-4-en-3,17-dione, a compound having the structure formula (I) depicted below: (Formula I) (I) useful as intermediate compound in the synthesis of the progestin compounds Desogestrel and Etonogestrel.
专利号:US-4277610-A 优先权日:1975-01-27 标 题 :Synthesis of 2,6,10-trimethyl-undecan-1-ol 发明人:COHEN NOAL; SAUCY GABRIEL 权利人:HOFFMANN LA ROCHE 摘要:A synthesis of 2,6,10-trimethyl-undecan-1-ol, an intermediate for producing vitamin E, from methacrolein, crotonaldehyde, β-hydroxy-isobutyric acid including intermediates in this synthesis.
摘要:Vashchenko, B. V.; Grygorenko, O. O., Science of Synthesis Knowledge Updates, (2021) 3, 346. 摘要:Vashchenko, B. V.; Grygorenko, O. O., Science of Synthesis Knowledge Updates, (2021) 3, 345.