新药盐酸美利曲辛的有机波谱分析

采用核磁共振波谱(NMR)、电喷雾质谱(ESI MS)、紫外(UV)、红外(IR)吸收光谱等技术确证新药盐酸美利曲辛的分子结构;应用NOE谱技术确定盐酸美利曲辛分子中芳香氢的各自化学位移信号;解释该结构在NMR、ESI MS、UV、IR等谱图中的特征吸收峰、共振峰及特征离子的一一对应归属.     

咪喹莫特的波谱学数据与结构表征

对咪喹莫特的红外(IR)、紫外(UV)、质谱(MS)、氢-氢相关谱(^1H--^1H COSY)、碳氢相关谱(HMQC)、碳氢远程相关谱(HMBC)予以解析并进行了报道。对所有的^1H NMR、^13C NMR谱的信号进行了归属；讨论了质谱的主要碎片离子的可能的裂解方式和红外特征吸收峰所对应的官能团的振动形式。     

辛伐他汀的波谱学数据和结构确证

对辛伐他汀的红外(IR)、紫外(UV)、质谱(MS)、氢-氢相关谱(^1H-^1HCOSY)、碳谱(^13C NMR,DEPT)、碳氢相关谱(HMQC)、碳氢远程相关谱(HMBC)予以解析并进行了报道,对所有的^1H NMR和^13C NMR谱信号进行了归属;讨论了红外特征吸收峰所对应的官能团的振动形式,并且对样品进行热差和热重分析,显示该样品为单一晶型,不含结晶水。     

meso-四(烷氧基苯基)卟啉及其金属络合物的波谱研究

采用^1H NMR、MS、IR、UV、元素分析等分析测试表征手段确证了所合成的10个系列卟啉及其金属络合物的结构,研究了不同位置、不同链长烷氧基四苯基卟啉和不同金属离子卟啉络合物的结构与^1HNMR、IR和UV等波谱之间的关系,总结了卟啉配体及其金属络合物的^1H NMR、IR和UV判据,报道和解释了meso-四(烷氧基苯基)卟啉铜、锰络合物和meso-四(邻烷氧基苯基)卟啉钴络合物的^1H NMR研究结果,通过MS、^1H NMR、IR、UV、元素分析确证了我们所合成的铁卟啉为μ-氧桥联夹心二聚体结构,且存在两种典型构象,导致同系列络合物有四种类型^1H NMR谱图。     

金雀花碱的波谱特征与结构确证

提供了金雀花碱结构的波谱特征。采用红外光谱(IR)、紫外光谱(UV)一维(1H,13C)和二维(1H-1HCOSY,HMQC,HMBC)核磁共振光谱(NMR)、质谱(EI-MS)对金雀花碱进行结构确证,对所有的1H NMR和13CNMR谱进行了归属;讨论了红外吸收光谱峰所对应的官能团的振动形式,并具体分析了金雀花碱MS中主要碎片离子的裂解途径。波谱学研究结果确证了金雀花碱的结构。     

依碳氯替泼诺的结构分析研究

对依碳氯替泼诺的红外光谱(IR)、紫外光谱(UV)、质谱(MS)、氢-氢相关谱(^1H-^1HCOSY)、碳谱(DEPT-45、DEPT-90、DEPT-135)、碳氢相关谱(HMQC)数据和解析进行了全面的报道。对所有的^1H NMR、^17C NMR谱的信号进行了归属，讨论了质谱的主要碎片离子的可能裂解方式和红外所对应的官能团的振动吸收形式、紫外特征吸收峰所对应的不饱和共轭体系电子跃迁能量。     

Petatrichol B： A Pentacyclic Triterpenoid with Unusual Skeleton from Petasites tricholobus

A novel pentacyclic triterpenoid, petatrichol B, was isolated from the rhizome of Petasites tricholobus. Its structure was established by means of spectroscopic analysis （EIMS, HRSIMS, IR, 1D NMR and 2D NMR）.     

美沙拉秦的波谱学数据与结构表征

对美沙拉秦的红外光谱（IR）、紫外光谱（UV）、质谱（MS）、碳谱（DEPT-135）、碳氢相关谱（HMQC）予以解析和报道.对所有1H NMR和13C NMR谱的信号进行了归属;同时讨论了质谱的主要碎片离子可能的裂解方式和红外特征吸收峰所对应的官能团的振动形式.     

尾式卟啉-5-氟尿嘧啶及其金属络合物的光谱分析

合成了24种新型的尾式卟啉-5-氟尿嘧啶化合物及其金属锰络合物,通过核磁共振氢谱（NMR）、质谱（MS）、红外光谱（IR）、紫外光谱（UV）及元素分析确定了其结构,并讨论了24种化合物光谱的关系特征及其规律,确定卟啉类配体与金属络合的NMR、IR、UV判据。     

拓扑异构体的研究(Ⅰ)C型与S型拓扑异构体的波谱性质及结构鉴定

利用 ¹H和 ¹³C NMR, IR, UV, SEM对合成的4种C型和S型拓扑异构体进行了结构表征和分析, 发现对于不同拓扑结构的C型和S型分子可以通过 ¹H NMR来鉴别, 而对于相同拓扑结构的S型cis(SC)和trans(ST)分子, C型 cis(CC)和trans(CT)分子则要结合 ¹³C NMR来鉴别. 四种拓扑异构体的IR, UV, 波谱性质以及SEM图象没有显著的差异.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.