微波作用下1,5-苯并硫氮杂-α-溴代-β-内酰胺衍生物的合成

1,5-苯并硫氮杂     

Synthesis of

A series of 1,1'-dicinnamoylferrocenes were converted to the corresponding [3]ferrocenophane diols (4a-e) in a stereoselective manner by using samarium diiodide to effect the intramolecular coupling reaction, aldol reaction, and reduction in one-pot operation. The major reaction pathway might be derived from a samarium chelated transition state (I(A)()) having the moieties of s-cis enone and (Z)-enolate. A solid-state structure of such [3]ferrocenophane diol product showed that the cyclopentadienyl groups were in an eclipsed orientation and slightly tilted.     

发散法合成树枝状高分子聚酰胺-胺

采用发散法,以乙二胺为原料,通过与丙烯酸甲酯和乙二胺进行Mickeal加成和酰胺化缩合反应,合成了以乙二胺为核、支化代为1.0的树枝状高分子聚酰胺一胺,讨论了反应温度、反应时间和投料摩尔比等因素对反应的影响,同时讨论了该反应的特点。结果表明：适宜的反应温度为25℃,反应时间为24h,投料比为mol0.5代PAMAM：mol乙二胺＝1：24,在此条件下,产品的产率为99.9%,纯度在995以上。     

多官能团分枝状化合物的合成研究：Ⅴ.多烯烃体系的合成

以六溴甲基苯为核心,季戊四醇三烯丙基醚为支化单元,采用收敛法合成了六方向,具有１８个末端烯丙基的多烯烃体系。     

N-酰基吡唑类化合物的制备及其在合成中的应用

N-酰基吡唑类化合物作为酰化试剂逐步引起了广泛关注,对其制备以及在醇解,氨解,格氏反应,瑞福尔马斯基反应等方面的用途做了探讨.     

制备方法对LaFeO3纳米粉体的影响

分别采用熔盐法和溶液燃烧法合成了钙钛矿型LaFeO3纳米粉体,系统研究了两种制备方法对粉体相结构、形貌的影响,用XRD、SEM和TG/DSC对纳米粉体进行了表征.结果表明:熔盐体系、煅烧温度、燃料类型和燃料/氧化剂的摩尔比对合成LaFeO3有重要的影响.450-750℃的熔盐NaNO2体系及650-800℃的熔盐NaN...     

烯胺酮的合成及其在有机合成中的应用

烯胺酮是目前应用较为广泛的有机合成中间体, 对其合成及其作为中间体在有机化合物特别是杂环化合物的合成中的应用进行了综述.     

均四嗪衍生物的合成

均四嗪衍生物在可见光区的最高吸收波长为500～550nm 之间,且由于其分子跃迁矩垂直于分子长轴,在液晶中显示负二向性,因而     

Synthesis of rodocaine

A new method for synthesis of rodocaine (1) is presented. Two key steps were carried out by the N-bromosuccinimide (NBS)-mediated intermolecular addition of known enamine 5 with allyltrimethyl silane in presence of boron trifluoride etherate (BF₃/OEt₂) and the intramolecular ring-closing metathesis of triene 3. The Diels-Alder cycloaddition of triene 3 with different ethyl propiolates was also studied.     

乙酰-DL-环己基甘氨酸的合成

以环己基溴为原料,在醇钠存在下,经过与丙二酸二乙酯发生烃化反应,再水解,酸化、脱羧制得环己基乙酸;后者再经溴化、氨解得到DL－环己基甘氨酸;最后在醋酐存在下发生乙酰化反应得到了环氧合酶－2（COX－2）抑制剂JTE－522的重要中间体乙酰－DL－环己基甘氨酸,目标产物结构经元素分析,IR和^1H NMR验证。     

N-羟基丁二酰亚胺的合成

N 羟基丁二酰亚胺是一种重要的有机中间体 ,可用于多肽合成中的外消旋抑制剂[1 ] 和一些抗菌素的合成 ,也可用于制备活性酯[1～ 3] 。近年来在生物活性分子的合成[4] 及乙烯型聚合物的分子量控制[5]上也获得了广泛的应用。N 羟基丁二酰亚胺的合成早已有报道[6] ,但收率较低。Hoppe Seyler′s[7] 以水和二氧六环作为丁二酸酐与羟胺反应的混合溶剂 ,加热环合脱水 ,然后用乙酸乙酯反复提取 ,虽可得到75 %收率 ,但产物中往往混有 5 %～ 1 0 %的丁二酸难以除去 ,若要获得商品级产物 ,后处理过程复杂 ,且要损失 1 5 %～ 2 0 %的产物[8] 。Cherut…     

白鲜碱的合成

以苯胺为原料经取代、关环、甲基化、还原、消除反应合成了呋喃喹啉类生物碱白鲜碱,总收率17%,其结构经1H NMR,13C NMR和MS确证.     

Synthesis of Octafluoroporphyrin

Despite the long list of known fluoroporphyrinoids, the most fundamental 2,3,7,8,12,13,17,18‐octafluoroporphyrin (OFP) has not been synthesized until now. It is achieved by condensation of two molecules of tetrafluoro‐dipyrrylmethane‐2‐carboxaldehyde in the presence of magnesium(II) salts. The fluorinated dipyrrylmethane also gives 5,15‐bis(pentafluorophenyl)‐OFP (F18P) with a reasonable yield. Both Mg/OFP and Zn/F18P in the solid‐state reveal an essentially flat structure. The fluoro groups impart as much as a 0.5 V anodic shift for porphyrin ring oxidation/reduction, as well as hypsochromic shifts in the Uv‐vis spectra.     

N-烃基-N′-取代苯基硫脲类化合物的合成

N-烃基-N′-取代苯基硫脲具有多种重要的生物活性,如抗结核、抗真菌、除草及促进植物生长等功效。为了进一步研究此类化合物的性质,以期得到有生物活性的化合物,我们以丙酮为溶剂,在三乙胺或三正丁     

双氯乙酸苯二酚酯的合成

以丙酮为溶剂、三乙胺为缚酸剂,苯二酚10mmol,n(苯二酚)：n(氯乙酰氯)=1.0：3．0,在0℃～5℃的冰水浴下反应30min后再加热回流4h～5h,合成了两个双氯乙酸苯二酚酯(收率分别为63．4％,70．2％),其结构经元素分析、1H NMR和MS确认。     

Synthesis of barettin

The indole alkaloid barettin (with bromine in 6-position), isolated from the marine sponge Geodia Barretti, has been synthesised via a Horner-Wadsworth-Emmons type reaction from 6-bromoindole-3-carboxaldehyde to introduce the dehydro-functionality. Subsequent deprotection and cyclisation afforded the natural product in Z-conformation.     

Synthesis of Tangutorine

Tangutorine ( 1 ) in the racemic form has been assembled from tryptamine and aldehyde 3 . The synthetic design was based on uncovering a hidden symmetry in the nontryptamine portion of the norketone 2 . A five‐step process with an overall yield of 7% was developed in which 2 was transformed into the target molecule via a Vilsmeier–Haack reaction and two reduction steps.     

Synthesis of platensimycin

In modern drug discovery, antibodies or libraries of simple synthetic organic compounds, mostly of heterocyclic origin, are favored. Natural products play an increasingly inferior role as they are considered structurally too complex, limited in quantity, and difficult to synthesize, manipulate, and derivatize. Thus it was a sensation when a Merck research group reported that classical screening of metabolites from Streptomyces platensis has unearthed a low-molecular-weight organic compound with remarkable antibiotic properties.