2,5-二取代基-1,3,4-噁二唑及噁二唑啉类化合物的合成

2-苯基-1,2,3-连三唑-4-甲酰肼(1)与芳酸在POCl_3催化下得到6种新的2-芳基-5-(2’-苯基-1’,2’,3’-连三唑-4’-基)-1,3,4-噁二唑(2)。1与羰基化合物缩合得到相应的酰腙(3),在Ac_2O作用下环化成2-取代基-3-乙酰基-5-(2’-苯基-1’,2’,3’-连三唑-4’-基)-1,3,4-噁二唑啉(4)。化合物的结构经元素分析,IR,~1H NMR和MS确证。     

2-取代亚肼基-1,3-二硫杂环戊烷类化合物的合成及其生物活性研究

以取代苯甲醛、取代吡啶和取代苯甲酸酯等为原料合成了 10种含硫杂环化合物 (其中 2a～ 2g化合物为国内外未见报道 ) .在合成过程中采用了超声波技术 ,极大地缩短了反应时间 ,提高了收率 .所得化合物的结构经IR ,1 HNMR ,MS和元素分析证实 .对其生物活性进行了初步测试 ,结果证明一些化合物具有良好的抑菌或杀菌作用 ,其中 2b ,2c ,2e ,2h ,2i和2j对大肠杆菌 ( 10 40 7号 )的抗菌效果与CET和SMZ相当 ;2b ,2c ,2f对草绿色链球菌 ( 112 3号 )的抗菌效果与CET和SMZ相当 .     

Dawson型磷钨钼杂多酸的制备及其对H2O2氧化环己酮制己二酸的催化

采用水热法制备了新型H6P2W9Mo9O62.24H2O催化剂,并用UV-Vis、FT-IR和TG-DTA等测试技术对催化剂进行了表征。以微波促进30%过氧化氢氧化环己酮制备己二酸合成反应为探针,考察了催化剂的催化性能。通过正交实验探讨了几种因素对反应的影响,确定了优化工艺条件为:n(环己酮)∶n(过氧化氢)∶n(草酸)∶n(催化剂)=100∶400∶1.25∶0.25,反应温度100℃,微波辐射功率400 W,反应时间3.5 h,己二酸产品的收率达87.33%,纯度可达99.7%。反应结束后,将反应后含催化剂的溶液浓缩至一定浓度,催化产率降低,重复使用5次收率降低为45.89%。     

4,5-二氧-2-硫-1,3,2,4-二氮二磷杂环戊烷的合成和结构

本文通过氨基甲酰基膦酰胺酯与4-(取代)苯基二氯化膦缩含,然后硫化的方法制备了一类新型的双磷杂环化合物——4,5-二氧-2-硫-1,3,2,4-二氮二磷杂环戊烷。利用HPLC分离出了顺式和反式异构体,并分别测定了其晶体结构。通过~1HNMR和~(31)P NMR谱研究了化合物的立体结构,顺式和反式异构体有不同的化学位移和偶合常数。生物测定初步结果表明,这些化合物都有一定的除草活性,其中个别化合物有较高的除草活性。     

磷钼钒杂多酸高效催化1,3-二氧杂环乙烷的合成

采用Dawson型磷钼钒杂多酸H8P2Mo16V2O62为催化剂进行了1，3-二氧杂环乙烷的高效合成．与传统的催化体系相比，该体系具有反应速度快、目标产物选择性高和反应条件更加温和等特点．     

新型2-(2'-取代亚肼基)-1,3-二硫杂环戊烷衍生物的合成和菌活性研究

通过结构改造并结合活性基团的拼接合成了11个未见文献报道的新型2-(2'-取代亚肼基)-1,3-二硫杂环戊烷类化合物,所有的目标物的结构都经HNMR,MS,IR和元素分析证实,选择了其中5个化合物对7种细菌进行了抑菌活性1测试,并与市售农药20%三环唑、70%威尔达甲托的抑菌活性进行对比,发现它们比市售农药有更为广泛的杀菌谱,对照农药只对金黄色葡萄球菌有良好的抑菌作用而这些化合物则对所选择的七个菌种均有良好的抑菌作用.其中化合物2-(对氟苯氧乙酰亚肼基)-1,3-二硫杂环戊烷(4c)的杀菌谱很广,它对金色葡萄球菌、大肠杆菌、白色念珠菌的抑杀活性都很好.     

2-(4′-吡啶甲酰亚肼基)-1,3-二硫杂环戊烷的合成

采用均匀设计对一种新型有机硫氮杂环杀菌剂——— 2_( 4′_吡啶甲酰亚肼基 )_1 ,3_二硫杂环戊烷 (异烟噻 )的合成工艺进行了优化 ,拟降低成本 ,提高收率 ,节省资源。对目标化合物的结构进行了元素分析和光谱分析 ,并初步测试了目标化合物的抑菌和杀菌效果。     

酒石酸水溶液中绿色合成5-芳基亚甲基-1,3-二噁烷-4,6-二酮衍生物

在酒石酸水溶液中,以芳香醛和1,3-二噁烷-4,6-二酮为原料,合成了14种5-芳基亚甲基-1,3-二噁烷-4,6-二酮衍生物,收率81%～95%,其中4f, 4g, 5f和5g为新化合物,其结构经¹H NMR, ¹³C NMR和MS(ESI)表征。并对反应条件进行了优化,对反应机理进行了探讨。     

1,3-偶极环加成合成新型含2-苯基-1,2,3-三唑基的1,2,4-噁二唑啉衍生物

Schiff碱 3和肟或氯代肟在三乙胺作用下通过 1,3 偶极环加成生成一系列含 2 苯基 1,2 ,3 三唑基的 1,2 ,4 二唑啉类化合物 4a～ 4g ,5a～ 5g和 6a～ 6g .2 1个新化合物的结构经元素分析 ,1 HNMR ,IR和MS谱确证 .     

3-取代胺甲基-5-连三唑基-1,3,4-噁二唑-2-硫酮的合成

2-苯基-1,2,3-三唑-4-甲酰肼(1)在CS_2/KOH作用下环化得到5-(2-本基-1,2,3-连三唑-4-基)-1,3,4-噁二唑-2-硫酮(2),2经Mannich反应合成得到标题化合物3-取代胺甲基-5-(2-本基-1,2,3-连三唑-4-基)-1,3,4-噁二唑-2-硫酮(3)。     

Synthesis of Novel 1,3-Dioxolane Nucleoside Analogues

Novel 1,3-dioxolane C-nucleoside analogues of tiazofurin 2-(2-hydroxymethyl-1,3-dioxolan-4-yl)-1,3-thiazole4-carboxamide as well as N-nucleoside analogues of substituted imidazoles 1-(2-hydroxymethyl-1,3-dioxolan4-yl)-4-nitroimidazole and 1-(2-hydroxymethyl-1,3-dioxolan-4-yl)-4,5-dicyanoimidazole were synthesized from methyl acrylate through a multistep procedure. Their structures were confirmed by IR,^1H NMR,^13C NMR spectraand elemental analysis.     

Preparation and Catalytic Activity of PW_(12)/PAn Material in Synthesis of 2-Methyl-2-Ethyl Acetoacetate-1,3-Dioxolane

Acetals and ketals are among the most important perfume materials and industrial materials of organic synthesis. Up to now, there are many methods to synthesize them. Conventionally H2SO4 is used as catalyst in factories, but it causes many problems, such as the erosion of equipment, difficulty for after-treatment, low quality of the products, etc. Heteropolyacids (HPA) and their salts have been extensively studied because of their interesting catalytic properties. Significant research effo…     

Synthesis of 4-Methyl-2-Isopropyl- 1,3 -Dioxolane by TiSiW12O40/ TiO2 as Catalyst

Acetals and ketals are a kind of the important compounds and used to protect carbonyl,middle material of the organic synthesis. What's more, they are a sort of the widely use flavor substance. 4-Methyl-2-isopropyl-1,3-dioxolane has fresh fruit odor and apple note. It is used to producing many sorts of essence. And the conventional method to synthesize 4-methyl-2-isopropyl-1,3-dioxolane makes use of sulfuric acid as catalyst in factories. But it causes many problems, such as the erosion of production equipment, difficulty after-treatment, low quality of the products, etc. HPA and its salts shows excellent catalytic activity to the esterification and have recently attracted much attention as catalysts for various industrial processes, because their acidic and redox properties can be controlled at atomic/molecular levels. Misono, Pope [1], and Wang [2]have reviewed the homogeneous catalysis and fine organic synthesis catalyzed by heteropoly compounds. However, there is no report on the synthesis of 4-methyl-2-isopropyl-1,3-dioxolane catalyzed by TiSiW12O40/TiO2. TiSiW12O40/TiO2 was prepared according to reference [3] and identified by means of IR and XRD. The reaction was carried out in a three-neck flask equipped with a stirrer, a reflux condenser, and a thermometer. A certain amounts of isobutyraldehyde,1,2-propanediol and the catalyst was heated to boiling and refluxed until no water flowed off. The purified product was analyzed by IR spectra and 1HNMR.In this paper, we report 4-methyl-2-isopropyl-1,3-dioxolane was synthesized from isobutyraldehyde and 1,2-propanediol in the presence of TiSiW12O40/TiO2. The factors influencing the yield of product and the optimum reaction conditions were discussed. The optimum conditions are molar ratio of isobutyraldehyde to 1,2-propanediol was 1:1.5, the quantity of catalyst was equal to 0.5% feed stock, and the reaction time was 1.0 h. TiSiW12O40/TiO2 was an excellent catalyst to synthesize 4-methyl-2-isopropyl-1,3-dioxolane and the yield can be up to 92.1%. IR spectra of 4-methyl-2-isopropyl- 1,3-dioxolane shows peaks at 1191,1100,1022,950 cm-1; 1HNMR (δH, ppm):4.65-4.67 (d, 1H, CH), 4.02-4.20 (m, 1H, CH), 3.81-3.92 (d, 1H, CH), 3.35-3.43 (t, 1H, CH),1.61～1.85 (m, 1H, CH), 1.14-1.29 (d, 3H, CH3), 0.96 (m, 6H, CH3); nD20=1.4135; b.p. 127-130 ℃.And we found that the catalyst can be utilized repeatedly, moreover, the catalytic activities of the catalyst are almost unchanged after it has been used five times. From the above results and discussion, we can see that the synthesis of 4-methyl-2-isopropyl-1,3-dioxolane catalyzed by TiSiW12O40/TiO2 instead of sulfuric acid has a great prospect of application.     

Studies on Synthesis and Biological Activities of Novel Triazole Compounds Containing 1,3-Dioxolane

IntroductionTriazole compounds have attracted muchattention having been used as high efficient andwide spectrum fungicide and plant growthregulator[1— 4] .The triazole compounds containtintg1 ,3- dioxolane have the remarkable prevention ofthe control over plant diseases[5] .Propiconazol anddifenoconazole are two important representatives.But the necessary intermediate for synthesizingpropiconazol depends on imports,which leads tothe cost of production and application too high.According to th…     

Synthesis and Structure Characterization of Novel Triazole Compounds Containing 1,3-Dioxolane

Five novel triazole compounds containing group 1,3-dioxolane were designed and synthesized by taking difenoconazole as the start compound and changing diphenyl ether for benzyl phenyl ether. Their structure swere confirmed by elemental analyses, ^1H NMR and IR spectra. The single crystal structure of 2-[-4-(2,4-dichlorophenylmethoxy] phenyl-2-(1,2,4-triazol-l-yl ) methane-I, 3-dioxolane was determined by means of X-ray diffraction. The preliminary bioassays showed that the synthesized compounds exhibited some activities of fungicides and plant growth regulators.     

Microwave Spectrum of 1,3-Dioxolane in the v=4-8 States of Hindered Pseudorotation

The microwave spectrum of 1,3-dioxolane (C₃H₆O₂) (8 GHz - 53 GHz) has been studied. We identified 247 b type transitions in the v=4, 5, 6, 7, 8 states of excited pseudorotation: rotational transition; vibration-rotation transitions between the v=5 and v=6 states and between the v=7 and v=8 states. Rotational constants, centrifugal distortion constants, and coupling constants between general rotation and hindered pseudorotation have been determined. The intervals _{v v'} between the pseudorotational energy levels have been evaluated: ₅₆=298,618 MHz and ₇₈=201,078 MHz.     

锰配合物催化1,3-丁二烯环氧化合成环氧丁烯

合成了N,N′-dimethyl-N,N′-bis(2-pyridylmethyI)ethane-1,2-diamine(mep)及其相应的锰配合物,并将其锰配合物用于1,3-丁二烯的环氧化反应,高选择性的合成单环氧化合物环氧丁烯,考察了各因素对反应的影响,在优化的条件下能达到90%左右的收率和大于99%的选择性.在该...     

杂多酸盐催化合成碳酸丙烯酯

以杂多酸盐为催化剂,尿素(1)和1,2-丙二醇(2)为原料合成了碳酸丙烯酯.考察了不同杂多酸盐的催化活性和影响反应的因素.较适宜的反应条件为: 1 500 mmol, n(1) ∶ n(2)=1 ∶ 2, w(钨硅酸锌)=2.0%,于165 ℃反应6 h,收率97.32%.硅钨酸锌重复使用5次后,收率仍高于90%.     

N—烃氧丙酰基四氢噻唑—2—硫酮的合成

在三聚氯氰存在下由烃氧丙酸与四氢噻唑-2-硫酮反应得到N-烃氧丙酰四氢噻哇-2-硫酮(2a-i),由2a,c-h与格氏试剂反应得到烃氧乙基苯基酮(3a,c-h).产物2a-i未见报道.