N-[2-(1H-吲哚-3)乙基]-2-乙酰噻唑-4-甲酰胺及其类似物的合成

N-[2-(1H-吲哚-3)乙基]-2-乙酰噻唑-4-甲酰胺是最近从海洋细菌中分离得到的一种新型的天然杀藻剂, 以D-丙氨酸为原料合成了该化合物, 并用类似的方法首次合成了它的类似物2, 3和4. 其关键步骤为通过将取代的4-噻唑甲酸制成混酐与色胺连接的偶联反应. 各中间体都通过¹H NMR和¹³C NMR得到证实. 最终产品通过¹H NMR, ¹³C NMR和HRMS证实, 与文献所报道相一致.     

光谱法分析乙丙共聚物的序列结构及链节比

用FTIR, 1 H NMR和 13 C NMR分析乙丙共聚物的序列结构与链节比. 通过对乙丙共聚物 1 H NMR, 13 C NMR和 13 C-1 H二维核磁共振谱的综合分析, 提出了与前人不同的归属, 并提出了不同位置碳原子积分面积相关性分析方法, 该方法避免了烦琐的理论计算, 可简便地得到乙丙共聚物的主要序列结构. 通过比较 1 H NMR和 13 C NMR计算乙丙共聚物中乙烯、 丙烯链节比, 表明可以用 1 H NMR代替 13 C NMR完成对乙丙共聚物中乙烯、 丙烯链节比的定量计算.     

含1,2,3-三唑环的α,γ-二酮衍生物的合成研究

以对氯氯苄为原料,经取代、1,3-偶极环加成和缩合反应得到含1,2,3-三唑环的α,γ-二酮衍生物,其结构经1H NMR、13C NMR以及MS确证。研究表明,该α,γ-二酮化合物存在酮醇异构现象,在溶液中其酮醇异构体比例近似为1∶8。     

由4-戊炔酸和5-己炔酸合成Muricatacin和6-乙酰氧基十六碳烷酸-5-内酯立体异构体

以4-戊炔酸和5-己炔酸为原料,Sharpless不对称双羟基化反应为关键步骤,分别以6~7步反应及33.5%~54.6%的总收率合成了muricatacin和6-乙酰氧基十六碳烷酸-5-内酯的四个立体异构体.它们的化学结构得到1H NMR,13C NMR,HR-ESI-MS和X射线衍射的表征,(-)-epi-muricatacin的绝对构型通过X射线衍射予以证实.     

β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯/冰片酯合成研究

以3,4-二羟基苯甲醛为起始原料, 经苄基保护、Darzens环氧化、Lewis酸开环、NaBH4还原、催化加氢脱保护得到β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯和β-(3,4-二羟基苯基)-α-羟基丙酸冰片酯, 所得化合物的结构通过1H NMR、13C NMR, IR, MS证实. 该方法操作简单、毒性低、产物易于纯化.     

铜催化的多组分反应合成二芳基炔丙胺类衍生物

以醛、苯乙炔和二芳胺为原料, 三组分一锅法合成了一系列二芳基炔丙胺类化合物. 产物的结构通过1H NMR, 13C NMR和HRMS证实.     

两种β-榄香烯烃基硒醚类化合物的合成、表征

将硒用N2·H2O还原为Se2 2-后与卤代烃反应得到对称二硒醚,然后将其用NaBH4还原,再与13-氯-β-榄香烯作用,得到两种β-榄香烯烃基硒醚.用1H NMR,13C NMR,IR以及HRMS等手段对产物结构进行了表征.     

二醋酸碘苯促进的芳酮类化合物羰基邻位乙酰化反应研究

以苯乙酮类化合物为原料,氧化锌(ZnO)为催化剂,二醋酸碘苯为氧化剂,通过对羰基邻位饱和sp3-C—H键的氧化与乙酰化,成功的构建出了α-乙酸基苯乙酮类衍生物,其结构经1H NMR和13C NMR得到了确认,并提出了可能的反应机理.     

固体酸Amberlyst 15催化合成3-吲哚取代的苯酞类化合物

室温下, 以吲哚和邻甲酰苯甲酸为原料, 通过Amberlyst 15 (15 wt%)催化的傅-克反应, 高产率合成得到一系列3-吲哚取代的苯酞类化合物. 并通过1H NMR, 13C NMR, 红外光谱, 高分辨质谱确证了产物的结构.     

新型2-芳氨基嘧啶衍生物的合成

通过间羟基苯硼酸与2,4-二氯嘧啶的Suzuki反应及其后酚羟基的烷基化得到4-芳基-2-氯嘧啶衍生物. 然后, 采用Pd(PPh3)4/dppf催化剂, 在温和的条件下实现了4-芳基-2-氯嘧啶类化合物和芳香胺的偶联. 合成了3个结构新颖的2-芳氨基嘧啶类化合物. 中间体及产物的结构均经由IR, 1H NMR, 13C NMR, MS和元素分析表征而予以证实.     

Furyl- and thienyl-silatranes and germatranes

We review our research on the synthesis and study of the physical and biological properties of furyl- and thienylgermatranes and -silatranes.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 725–732, June, 1992.     

Review and patents and literature

The use of the insect cell/baculovirus expression system for producing recombinant proteins of bacterial, plant, insect, and mammalian origin has become widespread. The popularity of this eukaryotic expression system is due to many factors, including (1) potentially high protein expression levels, (2) ease and speed of genetic engineering, (3) ability to accommodate large DNA inserts, (4) protein processing similar to higher eukaryotic cells (e.g., mammalian cells), and (5) ease of insect cell growth (e.g., suspension growth). The following review of the literature discusses two engineering aspects of recombinant protein synthesis by insect cell cultures: bioreactor scale-up and insect cell line selection. Following this review patent abstracts and additional literature pertaining to expression of recombinant proteins in insect cell culture are listed.     

多环芳二酐型聚酯亚胺膜的透气性能

多环芳二酐型聚酯亚胺膜的透气性能李悦生，丁孟贤，徐纪平（浙江大学高分子科学与工程研究所，杭州，３１００２７）（中国科学院长春应用化学研究所）关键词聚醚酰亚胺，聚酯酰亚胺，膜，透气性通常的聚酰亚胺加工性能较差，在芳环二酐的苯环间引入醚键等柔性基团后，其...     

微量元素与疾病诊断治疗的研究现状及展望

对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述，包括：微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。     

Preparation and photolysis of poly-p-ethylacrylophenone and poly-p-chloroacrylophenone and their copolymers with styrene and methyl methacrylate

Poly-p-ethylacrylophenone (PPEtAP) and poly-p-chloroacrylophenone (PPClAP) and their copolymers with styrene (PEtAP/S) and (PClAP/S) and with methyl methacrylate (PEtAP/MMA) and (PClAP/MMA) were prepared. Quantum yields of main-chain scissions at 366 nm at room temperature in benzene solution are of the same order as those of the unsubstituted polyacrylophenone and its copolymers. Substitution with chlorine and ethyl group in the para position compared to the unsubstituted polyacrylophenone and its copolymers leads to an increase of the lifetime for the n–π^* excited triplet state, as is evident from the measured quenching constants of photolysis. The low-temperature emission spectra of the copolymers are similar to the spectra of the model compounds in a polymer film. For the homopolymer, however, the character of the emission spectrum changes considerably.     

Concentrations and distributions of trace and minor elements in Chinese and Canadian coals and ashes

A total of 35 trace and minor elements including some of environmental significance were determined in each of a selection of 15 Chinese and 6 Canadian thermal coals and their ashes by using the SLOWPOKE-2 nuclear reactor facility of the University of Toronto. The concentrations and distributions of these constituents among the coals and their combustion products (viz. ash and volatile matter) are presented together with an interpretation of their significance in relation to the large scale combustion of these coals as thermal fuels in industrialized countries such as China and Canada. The detailed results showed wide variations in trace impurity concentrations (up to a factor of 100 and more) among the coals studied with few large differences between those of Chinese and Canadian origin except that the rare earths, Sc, Th, U, I, and Se were much higher in the former, other halogens, As and Na were lower. Values for elemental enrichment factors (EF) relative to normal crustal abundances indicated that only As(EF=13), Br(5.7), I(16), S(230), Sb(11) and Se(320) were appreciably enriched in coal. During static ashing at 750°C most of the halogens, S and Se were volatilized whereas most other inorganic constituents were highly retained and concentrated in the ash by factors of 6 to 11.     

Ground- and excited-state aromaticity and antiaromaticity in benzene and cyclobutadiene

The aromaticity and antiaromaticity of the ground state (S 0), lowest triplet state (T 1), and first singlet excited state (S 1) of benzene, and the ground states (S 0), lowest triplet states (T 1), and the first and second singlet excited states (S 1 and S 2) of square and rectangular cyclobutadiene are assessed using various magnetic criteria including nucleus-independent chemical shifts (NICS), proton shieldings, and magnetic susceptibilities calculated using complete-active-space self-consistent field (CASSCF) wave functions constructed from gauge-including atomic orbitals (GIAOs). These magnetic criteria strongly suggest that, in contrast to the well-known aromaticity of the S 0 state of benzene, the T 1 and S 1 states of this molecule are antiaromatic. In square cyclobutadiene, which is shown to be considerably more antiaromatic than rectangular cyclobutadiene, the magnetic properties of the T 1 and S 1 states allow these to be classified as aromatic. According to the computed magnetic criteria, the T 1 state of rectangular cyclobutadiene is still aromatic, but the S 1 state is antiaromatic, just as the S 2 state of square cyclobutadiene; the S 2 state of rectangular cyclobutadiene is nonaromatic. The results demonstrate that the well-known "triplet aromaticity" of cyclic conjugated hydrocarbons represents a particular case of a broader concept of excited-state aromaticity and antiaromaticity. It is shown that while electronic excitation may lead to increased nuclear shieldings in certain low-lying electronic states, in general its main effect can be expected to be nuclear deshielding, which can be substantial for heavier nuclei.