5－O－苯甲酰基－2，3－二脱氧－3－硝基－D－呋喃戊糖甲苷的合成研究

５－Ｏ－苯甲酰基－２，３－二脱氧－３－硝基－Ｄ－呋喃戊糖甲苷的合成研究史达清，周龙虎，高原，戴桂元（徐州师范学院化学系，徐州，２２１００９）关键词呋喃戊糖苷，Ｄ－木糖，异构化，合成５－Ｏ－苯甲酰基－２，３－二脱氧－３－硝基－Ｄ呋喃戊糖甲苷１是合成河豚...     

5－O－苯甲酰基－3－脱氧－3－硝基呋喃戊糖衍生物的异构化作用研究

５－Ｏ－苯甲酰基－３－脱氧－３－硝基呋喃戊糖衍生物的异构化作用研究戴桂元，史达清，周龙虎（徐州师范学院化学系，江苏徐州２２１００９）５－Ｏ－苯甲酰基－２，３－二脱氧－３－硝基－Ｄ－呋喃戊糖甲苷是合成河豚毒素的有用中间体￣［１］。我们在合成时发现了３－...     

铱配合物催化下炔基甲腙异构化反应的研究

铱配合物催化下炔基甲腙异构化反应的研究马春林（聊城师范学院化学系，聊城，２５２０５９）马永祥，陆熙炎（兰州大学化学系）（中国科学院上海有机化学研究所）关键词炔基甲腙，铱配合物，异构化反应，２Ｅ，４Ｅ－双烯基甲醛，１Ｚ，３Ｚ－双烯基偶氮化合物我们曾报道...     

3—甲基—4（1—吡咯烷基）苯基重氮氯化锌复盐的合成

３－甲基－４－（１－吡咯烷基）苯基重氮氯化锌复盐的合成唐有根蒋金芝＊刘春健（中南工业大学化学系长沙４１００８３）关键词重氮感光剂，甲基吡咯烷基苯基重氮氯化锌，合成１９９６－０９－０４收稿，１９９７－０３－３１修回光敏性重氮盐是非银感光材料中的一大类，...     

显色剂二溴硝基苯基重氮氨基偶氮苯与铜显色反应的研究及应用

本研究了显色剂二溴硝基苯基重氮氨基偶氮苯（简称ＤＢＮＤＡＡ）与铜显色反应的条件。结果表明：在ｐＨ５．４的六次甲基四胺－ＨＣｌ缓冲介质中在Ｔｒｉｔｏｎ－Ｘ－１００－ＳＤＢＳ存在下，ＤＢＮＤＡＡ与铜生成３：１的紫色稳定络合物，λｍａｘ＝５１６ｎｍ，ε５１６＝２．９×１０＾５Ｌ．ｍｏｌ＾－＾１．ｃｍ＾－＾１，铜量在０－１４μｇ／２５ｍｌ范围内遵循比耳定律，方法选择性好，可用于铝合金和硫铁矿中铜含量的测     

反相液相色谱法测定微量铬(Ⅵ)苯酚、4-硝基酚和十二烷基苯磺酸钠

１引言铬（Ⅵ）、苯酚和４－硝基酚是我国环境优先监测的工业污染物，其测定方法一直是环境分析中研究的重要课题。十二烷基苯磺酸钠（ＳＤＢＳ）是我国使用量最大的洗涤剂，它对环境造成的污染不容忽视。这４种物质有许多检测方法，但大多是用不同方法分别测定。本文建立了以甲醇、乙醚和ＨＡｃ－ＮａＡｃ缓冲溶液为流动相，反相高效液相色谱法分离和测定铬（Ⅵ）、苯酚、４－硝基酚和ＳＤＢＳ４种污染物的分析方法，并应用于环境水样中。２实验部分２．１仪器与试剂ＳＳＩ２２２Ｄ型高效液相色谱仪，ＵＶ－５００型紫外－可见检测器，Ｃｈ…     

离子电极法测定木糖

离子电极法测定木糖刘鹤，何亚明，胡伟凡（北京轻工业学院化工系北京１０００３７）关键词离子电极法，二硝基酚电极，木糖木糖常采用费林试剂法［１］，在沸腾条件下测定。当含量低于０．３％时，很难判断终点．本文用自制的２，４－二硝基酚电极，建立了测定木糖的离子...     

硝基化合物的硝基伸缩振动频率与取代基常数之间的关系

硝基化合物的硝基伸缩振动频率与取代基常数之间的关系丁金昌（温州师范学院化学系３２５００３）在硝基化合物的红外光谱中，重要的特征吸收峰是硝基的伸缩振动，人们曾对影响硝基伸缩振动频率的因素作了广泛的研究［１］。硝基化合物的硝基（ＮＯ２）伸缩振动频率的大小...     

4－硝基二苯胺合成方法的改进

４－硝基二苯胺合成方法的改进郭佃顺，黄汝骐，高蓉华，吴志广（山东师范大学化学系，济南２５００１４）４－硝基二苯胺是有机合成工业的重要原料和中间体，广泛用于橡胶助剂工业（如生产橡胶防老剂４０２０、４０１０ＮＡ等）和染料工业。４－硝基二苯胺通常由对硝基氯...     

偶氮染料的可见吸收光谱及发色效率

偶氮染料的可见吸收光谱及发色效率刘志杰，唐瑞仁，张建恒（西北大学化学系，西安７１００６９）重氮感光材料是目前非银盐感光材料中应用最广，技术较为成熟的一大体系，近年来在印刷、缩微、半导体工艺及办公室自动化等方面，广泛用来记录和传递信息￣［１］。根据重氮...     

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%.     

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.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

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.