2-(1-环己烯基)环己酮的合成

以酸或碱做催化剂，环己酮自身催化缩合生成以2-(1-环己烯基)环己酮为主的缩合产物，同时还生成2-环己亚烷基环己酮，以及副产物三聚物。考察了使用酸、碱在不同反应条件下的缩合反应，试验表明，硫酸做催化剂的工艺较为可取。     

离子交换树脂催化合成2-(1-环己烯基)环己酮

以环己酮为原料，利用双套管连续催化缩合反应及分离装置，在离子交换树脂催化下，制备2-(1-环己烯基)环己酮．考察了反应温度、反应时间、不同类型的离子交换树脂对2-(1-环己烯基)环己酮收率的影响．从而确定反应条件为：反应时间2．5h、反应温度85℃／2．0kPa，以HD-8型苯乙烯阳离子交换树脂为催化剂，在此条件下，2-(1-环己烯基)环己酮的收率达到85％以上．     

1-(2, 6, 6-三甲基-1-环己烯基-)-3-甲基-2-丁烯-4-醛合成新工艺

1-(2; 6; 6-三甲基-1-环己烯基-)-3-甲基-2-丁烯-4-醛合成新工艺;(三甲基环己烯基)甲基丁烯醛;卡宾反应; β-紫罗兰酮;三甲基溴化硫     

界面缩聚法合成双(烯基环戊二烯基)钛(锆)聚醚的研究

本文通过界面缩聚法利用双(烯基环戊二烯基)钛(锆)二氯化物与二酚反应,制成了16个新的高分子化合物,对它们进行了IR、TGA和分子量的测定。文中还对反应条件与分子量的关系进行了讨论。     

3-羟基-1-(2,6,6-三甲基-3-环己烯基)-1-丁酮的合成及其向卷烟烟气释放δ-突厥酮的研究

以亚异丙基丙酮,1,3-戊二烯为原料经Diets-Alder反应合成了4-乙酰基-3,5,5-三甲基环己烯(4),4再与乙酸乙酯在乙醇钠的存在下缩合得到1-(2,6,6-三甲基-3-环己烯-基)-1,3-丁二酮(5),5用硼氢化钠还原合成了3-羟基-1．(2,6,6-三甲基-3-环己烯基)-1-丁酮。其结构经GC—MS和^1H NMR证实。将此目标化合物用作香料成分加入卷烟,用GC—MS检测其烟气成分,发现此化合物在卷烟燃吸时能发生裂解反应,向烟气释放具有致香作用的δ-突厥酮。     

环状双(环戊二烯基)钛、双(甲基环戊二烯基)钛芳氧基衍生物的合成

在氨基钠存在下,二氯二茂钛或二氯二(甲基环戊二烯基)钛分别与2,2′—二羟基联苯、1,1′—二羟基—2,2′—联萘或间苯二酚等摩尔量反应,得到了四种新的环状有机钛芳氧基衍生物。而间苯二酚与二氯二(甲基环戊二烯基)钛反应,只得到单取代产物。新合成的衍生物都经元素分析、红外、核磁鉴定。     

(3-氮-吗啉)-1-(4-氯)-苯基-1-丙酮不对称还原产物光学活性的理论计算

采用AM1方法对(S)-4-苄基-5,5-二苯基-1,3,2-噁唑硼烷催化(3-氮-吗啉)-1-(4-氯)-苯基-1-丙酮不对称还原反应的立体控制步骤进行了计算,获得了R和S型过渡态的优化构型及其热焓和熵等热力学参数,计算得到了该步反应中生成R和S型对映体的反应速率常数之比,据此得到的不对称还原反应最终产物的光学活性e.e.的理论计算值,与实验结果相近.     

4-(4-吗啉)哌啶盐酸盐的合成

4-甲酸乙酯哌啶与溴苄反应,再经酰胺化和氨化反应制得关键中间体4-氨基-1-苄基哌啶(5);5与2,2-二溴二乙醚经环化反应制得N-苄基-4-(4-吗啉)哌啶,再经成盐,加氢合成了4-(4-吗啉)哌啶盐酸盐(1,总收率24.9%),1的结构经1HNMR,IR和GC-MS确认。     

3-芳基-3-环己烯基丙酸酯衍生物的合成和晶体结构

在KF-Al~2O~3催化下,将芳香醛、5,5-二甲基-1,3-环己二酮及丙二酸亚异丙酯在醇中反应,一锅式合成了一系列的3-芳基-3-(5,5-二甲基-3-羟基-2-环己烯-1-酮-2-基)丙酸酯。通过单晶X射线衍射分析确定了产物的结构,并提出了可能的反应机理。     

氯化铝高效催化合成1-(N-氨甲酸酯基)烷基-2-萘酚

无溶剂条件下,氯化铝可有效催化2-萘酚、醛和氨基甲酸酯三组分"一锅法"合成1-(N-氨甲酸酯基)烷基-2-萘酚。确定了较佳反应条件,产品经熔点、IR、1H NMR、元素分析进行表征。提出了可能的催化作用机理。     

Synthesis and characterization of new poly(N-1-adamantylmaleimide) and poly(N-1-diamantylmaleimide)

N-l-Diamantylmaleimide was synthesized by reaction of maleic anhydride with 1-aminodiamantane, followed by dehydration with acetic anhydride and sodium acetate. Poly(N-1-adamantylmaleimide) ( IIa ) and poly(N-l-diamantylmaleimide) ( IIb ) were polymerized using 2,2′-azobisisobutyronitrile (AIBN) as an initiator under different experimental conditions such as various initiator concentrations, solvents, polymerization temperatures, and polymerization times. Polymerizations of N-l-adamantylmaleimide in benzene at 60°C or in bulk gave polymers with molecular weights (2000–9500). The experimental results indicated that the propagation may be interrupted by steric hindrance of bulky and rigid substituents such as the adamantyl or diamantyl groups. In addition, the effect of chain transfer to monomer contributes to the relatively low activation energy. The glass transition temperatures of Ia and Ib were 204 and 216°C, respectively. The temperatures at 5% weight loss of the polymers IIa and IIb were above 412°C. © 1996 John Wiley & Sons, Inc.     

Interlayer-type Crystal Structure of N-（1-Adamantyl） urea

1 INTRODUCTION In the context of supramolecular chemistry, mo- lecules are joined together by intermolecular interac- tions to form a supramolecule whose physical pro- perties largely depend on the orientation and packing of molecules in the crystal structures[1]. The adaman- tane is a kind of cage alkane with high symmetry and stable framework. Its derivatives are extensively applied in the fields of medicine, macromolecular materials, aviation and so on due to the unique structures and …     

SYNTHESIS AND CHARACTERIZATION OF N-（1-NAPHTHYL） SUCCINIMIDE

In this paper a modified two-step procedure for synthesis of N-（1-naphthyl） suecinimide （NaS） was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The results show that the melting point of our product is 159 ℃-160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks （1705cm^-3/1779cm^-3）, which are found to be quite different from the documented data （rap 147℃ -149℃; IR C=0-1700cm^-3）. Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.     

N─苯基邻苯二甲酰亚胺和N─对甲苯基邻苯二甲酰亚胺的晶体和分子结构

报道一种新类型的有机电子晶体Ｎ－苯基邻苯二甲酰亚胺（１）（Ｃ＿（１４）Ｈ＿９ＮＯ＿２）和Ｎ－对甲苯基邻苯二甲酰亚胺（２）（Ｃ＿（１５）Ｈ＿（１１）ＮＯ＿２）的晶体和分子结构，（１）属正交晶系，空间群为Ｐｃａｂ，ａ＝７．６４９（４），ｂ＝１１．６５９（２），ｃ＝２３．７３９（３）Ａ，Ｖ＝２１１７．０Ａ￣３，Ｚ＝８，Ｄ＿ｃ＝１．４０１ｇ／ｃｍ￣３，Ｍ＿ｒ＝２２３．２３，μ＝０．８８５ｃｍ￣（－１），最终偏离因子Ｒ＝０．０５３，Ｒ＿ω＝０．０４８；（２）属正交晶系，空间群为Ｐｎａ２＿１，ａ＝７．６２４（２），ｂ＝１１．２３７（１），ｃ＝１３．８５６（２）Ａ，Ｖ＝１１８７．０　Ａ３，Ｚ＝４，Ｄ＿ｃ＝１．３２８ｇ／ｃｍ￣３，Ｍｒ＝２３７．２６，μ＝２．７６４ｃｍ－１，最终偏离因子Ｒ＝０．０３６，Ｒ＿ω＝０．０３２。晶体结构测定结果表明，邻苯二甲酰亚胺的内酰亚胺碳、氮、氧原子与其苯并环共平面。化合物（２）中的甲基碳原子与取代基苯环共平面，苯并酰亚胺平面与取代苯环平面间的夹角分别为５８．４°（化合物１）和５６．２°（化合物２）。     

N─苯基邻苯二甲酰亚胺和N─对甲苯基邻苯二甲酰亚胺的晶体和分子结构

报道一种新类型的有机电子晶体Ｎ－苯基邻苯二甲酰亚胺（１）（Ｃ＿（１４）Ｈ＿９ＮＯ＿２）和Ｎ－对甲苯基邻苯二甲酰亚胺（２）（Ｃ＿（１５）Ｈ＿（１１）ＮＯ＿２）的晶体和分子结构，（１）属正交晶系，空间群为Ｐｃａｂ，ａ＝７．６４９（４），ｂ＝１１．６５９（２），ｃ＝２３．７３９（３）Ａ，Ｖ＝２１１７．０Ａ￣３，Ｚ＝８，Ｄ＿ｃ＝１．４０１ｇ／ｃｍ￣３，Ｍ＿ｒ＝２２３．２３，μ＝０．８８５ｃｍ￣（－１），最终偏离因子Ｒ＝０．０５３，Ｒ＿ω＝０．０４８；（２）属正交晶系，空间群为Ｐｎａ２＿１，ａ＝７．６２４（２），ｂ＝１１．２３７（１），ｃ＝１３．８５６（２）Ａ，Ｖ＝１１８７．０　Ａ３，Ｚ＝４，Ｄ＿ｃ＝１．３２８ｇ／ｃｍ￣３，Ｍｒ＝２３７．２６，μ＝２．７６４ｃｍ－１，最终偏离因子Ｒ＝０．０３６，Ｒ＿ω＝０．０３２。晶体结构测定结果表明，邻苯二甲酰亚胺的内酰亚胺碳、氮、氧原子与其苯并环共平面。化合物（２）中的甲基碳原子与取代基苯环共平面，苯并酰亚胺平面与取代苯环平面间的夹角分别为５８．４°（化合物１）和５６．２°（化合物２）。     

N-(P-羟甲基苯基)咔唑丙烯酸酯的合成和聚合

<正> 为了深入认识含咔唑基单体的光敏性与聚合性的关系,在本系列含咔唑基化合物的基础上,合成了两个新单体:N-(p-羟甲基苯基)咔唑丙烯酸酯和N-(P-羟甲基苯基)咔唑甲基丙烯酸酯,并研究了其聚合行为。 化合物Ⅰ、Ⅱ、Ⅲ和聚合物的合成,反应式如下:     

Crystal and molecular structure of N-(1-silatranylmethyl)benzimidazole

The crystal and molecular structure of N-(1-silatranylmethyl)benzimidazole was established by X-ray diffraction. The coordination polyhedron of the silicon atom in this molecule is a trigonal bipyramid. The bond lengths and angles of the N-(1-silatranylmethyl)benzimidazole (SMBI) molecule are compared with the corresponding values for other derivatives of this heterocycle. The silatranylmethyl group, having a high electron-donor inductive effect, does not increase the total aromaticity of the SMBI molecule.     

Unusual course of the reaction of N-(tosylmethyl)thiourea and N-(azidomethyl)thiourea with sodium enolate of dimedone

The end product of the reaction of N-(tosylmethyl)thiourea or N-(azidomethyl)thiourea with sodium enolate of dimedone is bis(2-hydroxy-4,4-dimethyl-6-oxocyclohex-1-enyl)methane (methylenebisdimedone) instead of the expected 8a-hydroxy-7,7-dimethyl-2-thioxoperhydroquinazolin-5-one.M. V. Lomonosov State Academy of Fine Chemical Technology, Moscow 117571, Russia; Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 70–72, January, 2000.     

Structure of N-(1-silatranylmethyl) and N-(trimethoxysilyl-methyl) derivatives of nitrogen-containing heterocycles according to data of NMR, IR, and UV spectroscopy

The ¹H, ¹³C, ¹⁵N, and ²⁹Si NMR, IR, and UV spectra of N-(1-silatranylmethyl) and N-(trimethoxysilylmethyl) derivatives of nitrogen heterocycles have been studied. The dependence and interrelation of the chemical shifts of ²⁹Si and ¹⁵N nuclei of the silatranyl group in the spectra of N-(1-silatranylmethyl)-substituted nitrogen heterocycles are determined by the nature of the heterocyclic system. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 12, pp. 1857–1865, December, 2006.     

N-(1-萘基)琥珀酰亚胺玻璃态的晶化

采用X射线粉末衍射(XRD)和差示扫描量热分析(DSC)方法, 跟踪研究了N-(1-萘基)琥珀酰亚胺的液氮淬冷样品在室温(25 益)即在玻璃化转变温度以下的冷结晶行为. DSC和XRD的结果一致表明, 其冷结晶动力学曲线与熔融结晶完全不同, 呈现出“快-慢-快的三阶段增长趋势, 这一结果可以用低密度界面区成核和体积收缩效应给予解释.