微波辐射在合成沙利度胺中的应用

以邻苯二甲酸醉和尿素为原料,应用微波辐射加热技术,共经过四步合成目标产物沙利度胺的方法,且产物不需要经过多次纯化.考察了辐射功率、辐射时间、原料配比、溶剂用量等对收率的影响.与常规加热方法合成沙利度胺比较,微波辅助合成在提高产率的同时大大缩短了反应时间,且具有操作简单、环境污染小、产品质量好等优点.     

一步法合成沙利度胺及其重要的衍生物

沙利度胺（1）最早是由德国的一家制药公司在20世纪50年代上市的一种用于镇静和孕妇止吐的药物,当时被认为是一个毒性很小的药物,但是很快就发现这个药物有非常强的致畸性,于是在1962年这个药物撤出了市场。后期研究结果表明,沙利度胺的致畸性是由其5－异构体导致的,     

微波辐射催化合成肉桂酸苄酯

肉桂酸苄酯是一种具有弱苏合香、花香等香气的香料,主要用于配制龙蜒香,在东方型香脂中作为定香剂,也可用作皂用、化妆用及果实香精的调香配料。肉桂酸苄酯的合成,在工业上,主要采用肉桂酸钠与氯化苄在二乙胺作用下反应,反应时间长达17h,产率80％以上。近年来的研究     

微波辐射十六烷基三甲基氯化铵催化合成肉桂酸苄酯

以肉桂酸钠和氯化苄为原料,十六烷基三甲基氯化铵作催化剂,采用微波辐射技术,在常压下直接合成肉桂酸苄酯。最适宜的反应条件为：肉桂酸钠50mmol,n(肉桂酸钠)：n(氯化苄)=1．0：1．2,催化剂1．0g,微波功率300W,辐射时间25min,产率在84％以上。     

微波辐射下含四氢吡咯环C60衍生物的合成

以氨基酸、醛和C60 为原料在无溶剂条件下应用微波技术合成一系列含不同取代基的四氢吡咯环C60 衍生物 ,该反应在 8～ 10min内完成 ,产率 5 0 %～ 74%.     

水相中苯并噻唑类衍生物的微波辐射合成

在水相中建立了一种简单实用,廉价的2-碘芳胺与芳醛和硫氰酸钾反应生成苯并噻唑衍生物的微波辅助铜催化体系。该体系只需以碘化亚铜和1,10-菲罗啉为催化剂,以碳酸铯为碱的100 ℃水中反应30 min,就能得到大量苯并噻唑衍生物,最高产率达94%。     

微波辐射下2-取代苯并咪唑衍生物库的平行合成

以邻苯二胺及相应羧酸为原料,于多聚磷酸存在下,由微波辐射平行合成了一个小型2-取代苯并咪唑衍生物库,反应时间由常规加热的几小时到几天缩短为20min,且产率较高。经元素分析和1H NMR确证了产物结构。     

微波辐射下一步合成吡啶和吡喃衍生物

吡啶衍生物具有重要的生物活性 ,用作药物和农用化学品如ｈｅｒｂｉｃｉｄｅｓ[1 ] 。有些吡啶衍生物具有荧光性质 ,已被用于液晶工业。一些 2 氨基 4Ｈ吡喃具有光化学活性[2 ] 。多取代的四氢吡喃还是许多天然产物的基本结构单元[3] 。 4 芳基四氢吡喃可以转变成吡啶衍生物 ,后者是药物上重要的钙离子通道调节剂[4～6] 。自从ＳａｋｕｒａｉａｎｄＭｉｄｏｒｉｋａｗａ[7] 于 1 968年第一次报道在醋酸铵存在下丙二腈与α、β 不饱和酮反应得到吡啶衍生物以来 ,丙二腈与α、β 不饱和酮反应用于吡啶和吡喃衍生物的合成已愈来愈引起人们兴趣…     

新型含磺酰基的磷酰胺氮芥衍生物的合成

以磷酰胺氮芥为药效基团,对甲苯磺酰胺为载体,通过乙二胺的连接方式,合成了14个新型含磺酰基的磷酰胺氮芥衍生物,其结构经1H NMR,13C NMR,31P NMR和元素分析表征.     

无溶剂条件下微波辐射合成2-氨基噻唑衍生物

在无溶剂条件下, 用微波辐射法以碘、酮和硫脲为原料合成了9个2-氨基噻唑衍生物. 利用正交法优化了微波促进此类环化反应的最佳条件, 提出了微波条件下碘催化环化合成2-氨基噻唑衍生物可能的反应机理.     

微波无溶剂法合成香草醛氨基酸席夫碱

氨基酸席夫碱是制备特殊生物活性物质的重要中间体。氨基酸席夫碱中的亚胺(C=N)结构与亚磷酸烷基酯加成的化合物具有良好的抗植物病毒,除草,杀菌等性能[1-3]。氨基酸席夫碱中的羟基,羧基和亚胺等多个活性基团,可以与多种金属离子配位,其配合物具有抗菌,抗病毒,抗癌等性能[4-9],     

Fmoc-based solid-phase synthesis of adenylylated peptides using diester-type adenylylated amino acid derivatives

Phosphodiester-type adenylylated (AMPylated) Ser, Thr, and Tyr derivatives were developed for Fmoc solid phase peptide synthesis of AMPylated peptides. One-pot/sequential reaction consisting of condensation of an N-nonprotected adenosine derivative and Fmoc-Ser/Thr/Tyr-OAllyl using allyl-N,N-diisopropylchlorophosphoramidite and subsequent oxidation with m-chloroperbenzoic acid gave phosphotriester-type AMPylated Ser/Thr/Tyr derivatives. After Pd(0)-mediated deprotection of allyl groups, the resulting phosphodiester-type AMPylated Ser/Thr/Tyr derivatives were successfully incorporated into peptides by standard Fmoc solid phase peptide synthesis without significant side reactions including dehydroalanine formation.     

11-脱氧甘草次酸衍生物的合成

本文报道了具有潜在药理活性和应用前景的11-脱氧甘草次酸酯、11-脱氧甘草次酸盐的合成方法。     

Model studies on protease-catalysed peptide synthesis using 9-fluorenylmethoxycarbonyl protected amino acid derivatives

Summary Fmoc-Phe-OMe,Fmoc-Ala-OMe andFmoc-Gly-OH were coupled with H-Leu-NH₂ under catalytic action of chymotrypsin, papain and thermolysin, respectively. The influence of different reaction media and several reaction parameters, such as reactants and enzyme concentrations as well as reaction time, on the peptide bond formation was investigated. Abbreviations: IUPAC-IUB rules for peptides are followed, see (1984) Eur. J. Biochem.138: 9. All amino acids except of Gly are ofL-configuration.DMF=N,N-dimethylformamide,DTE=dithioerythritol,EDTA=ethylenediaminetetraacetic acid, disodium salt,N/C=ratio nucleophile component/carboxyl component,-OMe=methyl ester,TLC=thin layer chromatography.     

A novel method for the synthesis of polysubstituted diaminobenzonitrile derivatives using controlled microwave heating

A novel, simple and efficient method for the synthesis of polysubstituted diaminobenzonitriles has been developed that involves reaction of 1,1,3-tricyano-2-aminopropionitrile with nitroolefins under controlled microwave irradiation conditions.     

苯并异硒唑酮氨基酸衍生物的合成及抗脂质过氧化作用

在已知具有氧化作用的2-苯基-1,2-苯并异硒唑-3(2H)-酮(Ebselen)的基础上, 将其2-位苯环更换成氨基酸乙酯, 设计并合成了9个苯并异硒酮的氨基酸衍生物3～11. 这类化合物的抗氧化作用药理研究表明,它们对Fe^2^+/半胱氨酸及维生素C诱发的大鼠肝微粒体脂质过氧化有抑制活性, 部分化合物活性比母体化合物Ebselen更优.     

N-Alkylation of diethyl acetamidomalonate: synthesis of constrained amino acid derivatives by ring-closing metathesis

An efficient method for N-alkylation of diethyl acetamidomalonate (DEAM) is reported. C-Alkenylation was achieved by treating the N-alkenylated DEAM with various electrophiles in the presence of Cs₂CO₃. RCM reactions of C- and N-alkenylated products gave cyclic amino acid derivatives in good yields.     

Benzophenone Schiff bases of glycine derivatives: Versatile starting materials for the synthesis of amino acids and their derivatives

This review focuses on the introduction and early development, in solution, of phase-transfer catalyzed (PTC) reactions to afford racemic or enantioenriched natural and unnatural amino acids. To form monosubstituted amino acids alkylation reactions are performed on the benzophenone Schiff base of glycine. For α,α-disubstituted amino acids the activated intermediate is an aldimine derivative of the monosubstituted amino acid. Enantioenriched products are produced by organocatalysis using derivatives of Cinchona alkaloids as the phase-transfer catalyst. Selectivity for monoalkylatation and lack of product racemization depend on the acidities of the glycine imines, and dialkylated products are formed from aldimine esters of monoalkyl amino acids. The racemic and catalytic enantioselective reactions of a cationic glycine equivalent with organoboranes, organometallics and malonate anion are discussed as are other reactions of these versatile Schiff bases derivatives.     

Reaction of amino acid derivatives with C_(60)

Ammo acid derivatives react with C60 at 110-120℃to form adduct compounds.The products were isolated by column chromatography and were identified by FD-MS,UV-Vis,FT-IR and 13C NMR spectroscopies.