Preparation of new monomers aza-β-aminoacids for solid-phase syntheses of aza-β-peptides

The preparation of new N^β-Fmoc-protected aza-β³-amino acids (aza-β³-aa) with proteinogenic side chains as well as their N^β-Fmoc, N^β-Cbz or N^β-Boc aza-β³-amino esters (from Pro, Asn, Asp, Glu, Gln) by successive nucleophilic substitutions will be described.     

铕（Ⅲ）—β—二酮—4,5—二氮芴—9—酮三元配合物的合成

铕（Ⅲ）┐β┐二酮┐４，５┐二氮芴┐９┐酮三元配合物的合成成义祥徐端钧＊徐元植（浙江大学化学系杭州３１００２７）关键词铕，β－二酮，二氮芴酮，三元配合物，合成，荧光光谱１９９７－０３－３１收稿，１９９７－０７－１５修回噻吩甲酰三氟丙酮（ＴＴＡ）和苯甲...     

4—叔丁基—β—氯—α甲基肉桂醛的合成

从苯和叔丁醇出发，经过３步反应合成得标题化合物，总收率在６８％以上。     

A new approach to β-amino acids: biotransformation of N-protected β-amino nitriles

A number of novel N-protected β-amino nitriles were prepared as substrates for two nitrile-converting microorganisms, Rhodococcus sp. R312 and Rhodococcus erythropolis NCIMB 11540. The respective biotransformation products, β-amino acids, are known to be pharmacological very potent compounds.     

丙烯酸β-羧乙酯-苯乙烯共聚合的研究

<正> 丙烯酸酯类聚合物是一类性能优良的橡胶、涂料和粘合剂,酯的结构不同可得到性能各异的均聚物和共聚物。 丙烯酸β-羧乙酯(APA)是一种具有多种反应功能的丙烯酸酯单体,结构式为:CH_2=CH—COOCH_2CH_2COOH,其双键可发生加成聚合,制得的大分子带有反应性酯基和羧基侧基,以其制备反应性大分子具有广泛的应用前景。我们研究了丙烯酸β-羧     

Synthesis of a model system for the preparation of phloroglucinol containing natural products

A model system for the synthesis of phloroglucinol containing natural products was synthesized. Key steps include a manganic acetate-mediated cyclization and the facile conversion of an alkene into a β-bromoenone.     

Convenient procedure of Horner-Wadsworth-Emmons olefination for the synthesis of simple and functionalized α,β-unsaturated nitriles

A mild and practical procedure of Horner-Wadsworth-Emmons olefination promoted by lithium hydroxide and α-cyano phosphonates has been set up for the synthesis of α,β-unsaturated nitriles. The reaction conditions are tolerated by functionalized ketones and the exclusive formation of E-γ-hydroxy α,β-unsaturated nitriles has been observed.     

Normal-phase high-performance liquid chromatographic separations using ethoxynonafluorobutane as hexane alternative. II. Liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry applications with methanol gradients

We have reported recently that high-speed normal-phase (NP) HPLC separations of a broad range of organic compounds can be performed on cyano columns using gradients of methanol in hexane-like solvent-ethoxynonafluorobutane (ENFB), available commercially. In this communication, we demonstrate that atmospheric pressure chemical ionization (APCI) in combination with mass spectrometry (MS) can be effectively used for detection in such separations. The efficiency of APCI under conditions studied has also been compared to the efficiency of traditional electrospray ionization (ESI) in combination with MS for reversed-phase (RP) HPLC of the same compounds. The compounds included in this study were steroids, benzodiazepines, and other central nervous system-active substances, nonsteroidal anti-inflammatory drugs, tricyclic antidepressants, and beta-adrenergic blocking agents. Non-polar compounds were found to respond stronger when APCI-MS technique was used, whereas APCI and ESI ionization efficiencies were comparable when polar substances were studied. The combination of normal-phase HPLC separation conditions with mass spectral detection may expand the range of LC-MS applications traditionally associated with reversed-phase HPLC and ESI-MS detection.     

Silver (I)-promoted asymmetric halohydrin reaction of chiral N-enoyl-2-oxazolidinones: scope and limitations

The halohydrin reaction of chiral N-enoyl-2-oxazolidinones 1 by halogen (Br₂/I₂) and water were efficiently carried out in aqueous organic solvent promoted by silver(I) with high anti- and regioselectivity and moderate to good diastereoselectivities. The alkenoyl, cinnamoyl and electron-deficient cinnamoyl substrates smoothly underwent bromohydrin reaction in aqueous acetone but no iodohydrin reaction, where as electron-rich cinnamoyl substrates preferred to undergo iodohydrin reaction in aqueous acetone with moderate diastereoselectivity and enhanced diastereoselectivity was observed in aqueous THF.     

Synthesis of cyclopentane building blocks via an intramolecular CH insertion reaction of a chiral pool derived α-diazo-γ-hydroxy-β-ketosulfone

A highly functionalized cyclopentanone building block 13 was prepared by a facile Rh-catalyzed intramolecular CH insertion reaction of an enantiopure α-diazo-γ-hydroxy-β-ketosulfone 12, in turn derived from an α-hydroxy acid 2. A cyclic γ-hydroxy vinyl sulfone 16 was also prepared from 13.