微波辅助RGD环肽的固相合成

以2-氯代三苯甲基氯树脂为载体，采用Fmoc/t-Bu/Dmab正交保护策略，在微波辅助下合成了环肽c(fKRGD)，收率22.5%，纯度94.5%，其结构经MS(ESI), MS(MALDI-TOF)和HPLC确证。     

微波促进催产素和赖氨加压素环肽的固相合成

以Rink Amide-MBHA树脂为载体, 采用Fmoc/tBu正交保护固相合成策略, 运用微波照射促进, 先快速高效地合成得到载有催产素或赖氨加压素还原型多肽的树脂, 再将连接在树脂上的各还原型多肽分别在微波促进条件下和常温条件下环合形成二硫键制得环肽, 最后用Reagent K试剂将环肽从树脂上裂解下来得到目标多肽的粗品. 利用HPLC法测定不同固相环合条件下得到的多肽粗品纯度, 结果显示经微波促进固相环合得到的多肽粗品纯度明显高于常温条件下得到的多肽粗品纯度. 粗品最后经过反相制备高效液相系统纯化并冻干得到目标多肽纯品, 通过电喷雾质谱法测定了制得的还原型多肽及相应环肽的分子量, 验证了它们的结构.     

层状金属氧化物的固相合成及性质研究

许多具有层状结构的物质只在二维方向上存在强的化学键,相邻层之间以范德华力、氢键及静电等较弱的力结合.目前,交联粘土的研究正是致力于以交换或插入方法扩大层间距,增大表面积来制备大孔分子筛以满足大直径有机分子的催化、吸附等应用要求.但是,交联粘土的热稳定性较差,很难适应于工业生产对催化剂的要求,为此,对层状原料的开发研究得到人们的普遍重视.本研究利用固相反应,以适当的金属盐和氧化物为原料,经过高温焙烧制备出性能优良的层状金属氧化物.     

Sansalvamide A固相合成新方法

报道了Pd催化丁基二乙基硅烷树脂与N-Boc-4-溴代苯丙氨酸甲酯直接反应形成Si—Ar键一步构建出硅基连接分子的新方法, 并采用Boc策略增长肽链, 以PyBOP (benzotriazole-1-yl-oxy-tris-pyrrolidino-phosphonium hexafluoro- phosphate)为环合剂固相合成了sansalvamide A.     

纳米氧化镍的固相合成

纳米氧化镍的固相合成;NiO;纳米粒子;固相反应;合成机理     

糖肽的固相合成

目前糖肽的固相合成可以分为两种策略：构建单元策略和固相糖基化策略。本文对O-连接和N-连接糖肽固相合成的研究进展进行了综述。     

环六肽Thermoactinoamide A的固相合成及其抗菌活性

采用固相-液相两步法合成一种天然抗菌环肽Thermoactinoamide A。在9-芴甲氧羰基(Fmoc)固相合成的基础上,通过优化N,N-二异丙基乙胺(DIPEA)的添加量,得到直链肽,收率为84%,在此基础上,采用液相环合的方法对直链肽进行环合,通过优化环合体系中混合液的配比、初始pH等条件,得到Thermoactinomide A,收率为51%,总收率43%。抑菌实验结果表明,Thermoactinoamide A对金黄色葡萄球菌的最小抑菌浓度为32μg/m L。固相合成与液相环合两步法合成步骤少、过程简单、产率较高,为进一步研究该天然产物的生物活性及构效关系奠定了基础。     

糖肽的固相合成

综述了固相法合成糖肽的最新进展，论述了合成策略和所用聚合物载体，这是一种很有前途的合成糖肽的方法，参考文献４２篇。     

微波固相合成氧化锌纳米棒

通过前驱体的微波固相热分解法快速合成了氧化锌纳米棒, 其直径在60～385 nm之间, 长可达数微米. 前驱体则通过一步室温固相反应制备. 用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、能量色散X射线分析(EDX)和透射电子显微镜(TEM)对产物的结构和形貌进行了表征. 同时, 对氧化锌纳米棒的光致发光(PL)性能作了测试, 结果表明在355 nm处有一个明显的近带隙发射峰. 另外, 对比实验表明, 微波辐射在氧化锌纳米棒的形成过程中起了关键性作用, 并对其形成机理进行了初步探讨.     

抗肿瘤环八肽Samoamide A的固相合成及其细胞毒性

采用Fmoc固相合成法,以2-氯三苯甲基氯（CTC）树脂为固相载体,Fmoc保护的氨基酸为原料,合成了环八肽Samoamide A,其结构经¹H NMR, ¹³C NMR和LC MS（EI）确证。研究了反应溶剂、缩合剂、切割条件和pH对Samoamide A收率的影响。结果表明：合成Samoamide A的最佳条件为：60%DCM/DMF为溶剂,O-苯并三氮唑-N,N,N′,N′-四甲基脲四氟硼酸(TBTU)为缩合剂,TFA/EDT/PhOH/H₂O/硫茴香醚为切割试剂(80/2.5/7.5/5/5, V/V/V/V/V), pH 8.0,总收率54.5%。采用MTT法研究了Samoamide A的细胞毒性。结果表明：Samoamide A浓度为50.0 μg·mL^-1时,4T1细胞的存活率为20.79%。     

Solid-phase synthesis of Mannich-base hybridized cyclopeptides

A synthesis of new cyclopeptides is reported via Mannich condensation on solid support with a simple work-up procedure and very good yields.     

Synthesis of Nitrogen-containing Cyclopeptides from N-Terminal Lysine Precursor on Solid Supports

Three synthetic routes for the preparation of nitrogen containing cyclic compounds have been developed, in which the assembling of Fomc-Lys(Boc) residue at N-terminal of resin-bound intermediates is a key prerequisite. Six peptides with nitrogen containing local cyclic structure were efficiently synthesized in good yield starting from chloromethyl resin.     

环肽的合成研究进展

对环肽进行了分类, 并对具代表性的经典型、DKP (Diketopiperazine, 哌嗪二酮)型、醚桥型、烯桥型、单硫及多硫醚型、刚性桥型、仲(叔)胺型、Mannich碱型、联苯型及Freidinger型环肽的合成方法逐一进行了描述.     

新型含二硫键的环肽的合成

本实验设计从Boc-Glu-OH,Boc-Asp-OH的两个羧基出发,最后通过I2氧化两个半胱氨酸的巯基生成二硫键,得到一类新型含二硫键的环肽,该环肽通过1H NMR,MS等确定了其结构.     

An Efficient Synthesis of Cyclopeptides Bridged with Aliphatic-aryl Ether Bond

Based on the pseudo-dilution effect (PDE) on solid support, three cyclopeptides with an aliphatic-aryl ether bond as the bridge were synthesized via SN2 reaction between bromoacetylated at N-terminal and the phenol -OH group in C-terminal Tyr residue. All the products were obtained in good overall yields and characterized by related analytic data.     

Nitrogen-Containing Six-Membered Heterocycles: Solid-Phase Synthesis

Solid-phase organic synthesis is a rapidly expanding area of synthetic chemistry that is being widely exploited in the search for new medicinally important compounds using combinatorial techniques. In recent decades, a large number of reports related to solid-phase synthesis of heterocycles have appeared because of the wide variety of their biological activity. In this review, we report the important role of solid-phase synthesis in the synthesis of nitrogen containing six-membered ring heterocycles.     

Solid-Phase Synthesis of Nitrogen-Containing Five-Membered Heterocycles

In recent decades, a large number of reports related to solid-phase synthesis of heterocycles have appeared, owing to the wide variety of their biological activity. This review introduces the key concepts of solid-phase methodology and combinatorial synthesis with particular focus on the important role of solid-phase synthesis in the synthesis of nitrogen-containing five-membered ring heterocycles.     

Solid-Phase Synthesis of N-Aryl Succinimides

A new method upon adopting a solid-phase strategy for synthesis of N-aryl succinimides is described here, using the silica-bound benzoyl chloride (SBBC) as dehydrating agent in reaction with N-arylsuccinamic acids. The main advantage of this method is the recyclability of SBBC.