1,2-二溴-2-甲基丙烷置于氢氧化钾体系中,用 乙二醇 用作溶剂,以80%的收率获得1-溴-2-甲基-1-丙烯 参考文献:Synthesis Of The Stereoisomers Of A Novel Antibacterial Agent And Interpretation Of Their Relative Activities In Terms Of A Theoretical Model Of The Penicillin Receptor 标题:Synthesis Of The Stereoisomers Of A Novel Antibacterial Agent And Interpretation Of Their Relative Activities In Terms Of A Theoretical Model Of The Penicillin Receptor 摘要:2,2-二甲基-3-(2'-羟丙基)-5-羧基-δ3-1,4-噻嗪(1)是一种设计的抗菌剂.根据对青霉素与青霉素结合蛋白模型的复合物如何反应的分析,1含有一个功能基团(c=n),可以根据假定的反应enz-Oh + C = N-> Enz-O-C-Nh与受体的丝氨酸羟基反应.化合物1还包含额外的取代基,旨在将o-H和c=n基团相对于酶-底物复合物中的位置设计成一种几何构型,试图重现两种反应物的最佳接近几何构型.一个最重要的假设是这种最佳几何构型可以从头计算.在对1的第一次制备中,(+/-)-5-甲基-4-己烯-2-醇(2)被转化为(+/-)-2-巯基-2-甲基-5-叔丁基二甲基硅氧基-3-己酮(7)的锂盐,然后与n-叔丁氧羰基-D-和l-丝氨酸-β-内酯(3)缩合.合成完成后,用甲酸去保护,然后在水中环化.2的r和s对映体现已被获得,并通过r-和s-丙烯氧化物与由β,β-二甲基乙烯基溴制备的有机金属试剂反应,确定了醇的绝对构型.R醇也通过脂肪酶催化的三氟乙基丁酸酯转酯化和三氟乙基酯的化学水解获得.2的r和s对映体转化为7的r和s对映体,然后与3的r和s对映体缩合,以在约95%光学纯度形式中产生化学不稳定的1的各立体异构体.抗菌活性存在于5S,8R和5S,8S异构体中.这些发现与理论模型一致.希望可以改进引物结构1的稳定性,以便进行与识别青霉素的酶的结合实验. Doi:10.1139/v94-134
专利号:US-9126995-B2 优先权日:2011-11-08 标题:Method for catalytic asymmetric synthesis of optically active isoxazoline compound and optically active isoxazoline compound 发明人:TOYAMA KEN-ICHI; MORIYAMA YUJI; MATOBA KAZUTAKA; YAOSAKA MANABU; IKEDA EITATSU 权利人:NISSAN CHEMICAL IND LTD 摘要:There is provided a method for catalytic asymmetric synthesis of optically active isoxazoline compound and an optically active isoxazoline compound. A method for catalytic asymmetric synthesis of optically active isoxazoline compound of a formula (6) including reacting an α,β-unsaturated carbonyl compound of a formula (1) and a hydroxylamine in a solvent in the presence of a base by adding a chiral phase transfer catalyst. An optically active isoxazoline compound of a formula (13) that can be synthesized by the method.
专利号:US-5780579-A 优先权日:1993-08-10 标题:Method for the preparation of polyamino acids 发明人:SOULA GERARD; GROSSELIN JEAN-MICHEL; JORDA RAFAEEL; CASTAN CATHERINE 权利人:FLAMEL TECH SA 摘要:PCT No. PCT/FR94/00992 Sec. 371 Date Mar. 28, 1996 Sec. 102(e) Date Mar. 28, 1996 PCT Filed Aug. 9, 1994 PCT Pub. No. WO95/04772 PCT Pub. Date Feb. 16, 1995The present invention relates to a method for the preparation of polyamino acids, with controlled molecular weights, by polymerization of N-carboxyanhydrides (NCAs) of at least one amino acid, using at least one initiator of the strong base type and in liquid medium, characterized in that it consists in including, in the liquid reaction medium, given amounts of water and/or of alcohol. Application: synthesis of polyamino acids with mechanical and rheological characteristics adapted to applications as biomaterials.
专利号:US-4503232-A 优先权日:1982-04-24 标题:Method for the preparation of α-ketoamide imines 发明人:KOBAYASHI TOSHIAKI; TANAKA MASATO 权利人:AGENCY IND SCIENCE TECHN 摘要:The invention provides a novel method for the preparation of an alpha -ketoamide imine having a characteristic structure expressed by the formula in which R is a group such as an alkyl, aryl or the like group, in a one-step reaction in which a halogen-containing organic compound reacts with a primary amine and carbon monoxide in the presence of a carbonylation catalyst. The product compound is useful as an intermediate for the synthesis of various kinds of organic compounds including medicines and agricultural chemicals.
专利号:US-5596123-A 优先权日:1992-11-25 标 题 :Boric ester synthesis 发明人:ELGENDY SAID M A; DEADMAN JOHN J; PATEL GEETA; GREEN DONOVAN S; BABAN JEHAN A; KAKKAR VIJAY V; CLAESON GORAN K 权利人:THROMBOSIS RES INST 摘要:Stable alpha -substituted boronic esters, e.g. for use in peptide synthesis, are prepared by reacting a substituted alkene of the formula: with a disubstituted borane of the formula: wherein: (i) R1 and R2 are each selected from various groups which are preferably not leaving groups; (ii) X is halogen or other leaving group; (iii) Y is H or lower alkyl; (iv) Q1 and Q2 are each selected from various groups which are preferably such that the borane is non-hydrolyzable, and particularly Q1 and Q2 together may represent a residue of a diol such as catechol or pinanediol.
专利号:US-2014350261-A1 优先权日:2011-11-08 标 题 :Method for catalytic asymmetric synthesis of optically active isoxazoline compound, and optically active isoxazoline compound
专利号:CN-110483289-A 优先权日:2019-07-31 标题 :A kind of method for asymmetric synthesis of chiral alkenoate