3-甲基-4-氨基-5-巯基-1,2,4-三唑衍生物的合成及抗真菌活性

以3-甲基-4-氨基-5-巯基-1，2，4-三唑为起始原料，与卤代苄基在无水乙醇中回流制得中间体3-甲基-4-氨基-5-苄硫基-1，2，4-三唑，再与2，4-二氯苯甲醛在醋酸回流下缩合，即制得相应的目标化合物三唑席夫碱。利用1^HNMR和元素分析确证了中间体和目标化合物的结构。选择7种真菌为实验菌株，对中间体和目标化合物进行体外抑菌活性测试。     

4-乙酰氧基-2-甲基-2-丁烯-1-醛的合成方法

总结了维生素A的关键中间体4-乙酰氧基-2-甲基-2-丁烯-1-醛的合成方法，对各种合成方法的特点作了简要介绍，并且分析了主要合成方法的优缺点。     

2-[7-氟-4-（3-碘-丙-2-炔基）-3-氧-3,4-二氢-2H-苯并嗯嗪[b][1,4]-6-基]-4,5,6,7-四氢-2H-异吲哚-1,3-二酮的合成

标题化合物（B2055）是具有较高原卟啉原氧化酶抑制剂除草活性的N-苯基酞酰亚胺类新化合物，合成该化合物的关键步骤是2-[7-氟-4-（丙-2-炔基）-3-氧-3，4-二氢-2H-苯并曝嗪[b][1，4]-6-基]-4，5，6，7-四氢-2H-异吲哚-1，3-二酮（丙炔氟草胺，flumioxazin）的碘化。为寻求更经济和可工业化的合成路线，考察了不同的碘化剂、溶剂、原料配比、反应温度及反应时间对丙炔氟草胺的转化率和产品B2055收率的影响，在以醋酸为溶剂，氯化碘为碘化剂，原料丙炔氟草胺与氯化碘的物质的量比为1：3，反应温度为20℃，反应时间为60min的工艺条件下，原料丙炔氟草胺转化率为92．2％，产品B2055收率为90．7％。     

6-硝基-1,2-重氮氧基-4-萘磺酸及其杂质的高效液相色谱分析

本文以反相高效液相色谱对6-硝基-1，2-重氮氧基-4-茶磺酸及有机杂质进行了分析，选择了流动相、离子对、检测波长，研究了不同牌号ODS C18色谱柱的重现性，得到了6-硝基-1，2-重氮氧基-4-萘磺酸及杂质(1，2-重氮氧基-4-萘磺酸、8-硝基-1，2-重氮氧基-4-萘磺酸)的相关系数分别为：0.99956、0.99991、0.99317；标准偏差和变异系数分别为：0.214250％、0．016890％、0．564557％、0.012695%、0.488467％、0.014560％得到了准确度数据，确定了最小检出量。     

3-氯-4-（2-溴甲基-4-甲基-1，3-二恶戍烷-2-基）苯基-4’-氯苯基醚的合成

3-氯-4-（2-溴甲基-4-甲基-1，3-二恶戍烷-2-基）苯基-4’-氯苯基醚是杀菌剂苯醚甲环唑的一个重要中间体。以2-氯-4-（4-氯苯氧基）-苯乙酮为起始原料，采用溴化和合环同时进行的合成工艺制得该化合物，收率90％．产品含量95％。优化了反应条件，简化了操作。     

4-氨基-3-肼基-5-巯基-1,2,4-三唑的合成及其对醛的检验

以硫脲和水合肼合成了可用于检验醛的试剂——4-氨基-3-肼基-5-巯基-1，2，4-三唑(别名：紫醛)，其结构通过红外光谱、核磁进行了确定。试验表明，紫醛对醛的检验敏感、专一、快速、操作简单。     

（R）-3-（3-氟4-吗啉苯基）-2-氧-5-噁唑烷基甲醇的合成

以3，4-二氟硝基苯为原料，与吗啉在二异丙基乙胺中反应4h得到3-氟-4-吗啉硝基苯(Ⅰ)，在w(Pd)：10％催化下，Ⅰ与甲酸铵在V(THF)：V(甲醇)=1：4中反应6h，得3-氟-4-吗啉苯胺(Ⅱ)，Ⅱ与光气在通入干燥HCl气体下反应得3-氟-4-吗啉异氰酸苯酯(Ⅲ)，最后在无水LiBr和n-Bu3PO催化下，Ⅲ与(R)-丁酸缩水甘油酯在二甲苯中反应2h，所得产物在甲醇钠催化下，与甲醇反应3h，合成了(R)-3-(3-氟-4-吗啉苯基)-2-氧-5-噁唑烷基甲醇(Ⅳ)，总收率35．8％。     

对甲苯磺酸催化合成4-苯基-6-甲基-5-乙氧羰基-3，4-二氢嘧啶-2（H）-酮

研究了对甲苯磺酸催化合成4-苯基-6-甲基-5-乙氧羰基-3，4-二氢嘧啶-2（H）-酮，并得出最优工艺条件：对甲苯磺酸用量0．8g，反应温度70℃，反应时间50min，n（苯甲醛）：n（乙酰乙酸乙酯）：n（尿素0．0375moI）为1，0：1．2：1．5，此条件下产率为86．9％。     

1-（6-甲氧基-2-萘基）丁-1，3-二酮的制备

简化和改进了1-(6-甲氧基-2-萘基)丁-1，3-二酮的制备方法。以2-乙酰基-6-甲氧基萘为原料，与乙酸乙酯反应制备目标产物，总收率81．6％。该方法原料易得、操作简单、成本降低，并实现了工业化生产。     

（S）-5-苄基-2，2，3-三甲基-4-硫咪唑烷酮的制备方法

成功研究了以P2S5／Al2O3体系作为硫代试剂，将（S）-5-苄基-2，2，3-三甲基-4-氧咪唑烷酮转化为（S）-5-苄基-2，2，3-三甲基-4-硫咪唑烷酮的方法，且反应条件温和，收率较高。     

稻茬免（少）耕小麦田除草技术试验研究

1995～1996年在稻茬免耕小麦田,进行了播前和播后药剂除草试验.结果表明,播前用41%草甘膦75ml/667m~2或20%百草枯100ml/667m~2防除杂草效果分别为96、94.1%.播后4天用10%甲黄隆4g/667m~2、10%甲黄隆4g/667m~2+25%异丙隆100g/667m~2.对总草株防效分别61.4、80.3%,明显优于50%丁草胺100ml/667m~2防效(44.2%).而在小麦苗2叶1心期用10%甲黄隆4g/667m~2、10%甲黄隆4g/667m~2+25%异丙隆100g/667m~2、10%甲·绿5g/667m~2、25%异丙隆250g/667m~2,对总草株防效分别达82.6、97.3、90.0、88.3%.且比播后土壤处理防效好,并对小麦较安全.示范推广应用中,将播前和播后药剂除草技术相结合,可有效控制稻茬免(少)耕小麦田草害.     

纳米SiO2填充LLDPE复合材料耐热性的研究

采用DSC方法研究了纳米二氧化硅(SiO2)填充线性低密度聚乙烯(LLDPE)的熔融特性。结果表明：填充LLDPE的高温熔融峰峰值温度Tm2变化不大，低温熔融峰温Tml则随着纳米SiO2用量的增加明显向低温偏移，显示出纳米粒子的异相成核作用；在纳米SiO2用量相同的情况下，与表面未处理SiO2及经表面偶联剂处理纳米SiO2填充体系相比较，加有大分子相容剂的体系的Tml和Tm2均有所下降，同时熔融峰宽化；填充LLDPE的热变形温度HDT和软化温度Tg均随纳米SiO2用量的增加而提高；与表面未处理填充体系相比，硅烷偶联剂处理纳米SiO2填充体系的HDT有所上升，加有大分子相容剂的体系的HDT上升则更为明显。     

白炭黑补强溴化丁基橡胶的性能及特点

研究了白炭黑补强溴化丁基橡胶（BIIR）的性能及特点。结果表明；与炭黑补强相比，白炭黑补强的BIIR表现出了良好的工艺性能、力学性能和热老化性能；硅烷偶联剂（Si69）用置对硫化胶的力学性能有很大的影响；同时还发现白炭黑补强BIIR的拉伸应力软化效应和应力松驰性能与炭黑补强BIIR有着明显的区别。     

急性冠状动脉综合征患者血清中基质金属蛋白酶-2的表达

目的探讨急性冠状动脉综合征与血清基质金属蛋白酶-2(MMP-2)的相关性。方法应用酶图(SDS-PAGE en-zymograph)和Western blot方法检测50名急性冠脉综合征患者(27名ST段抬高急性心肌梗塞患者和23名不稳定性心绞痛患者)、20名稳定性心绞痛患者及40名正常对照者的血清MMP-2水平。结果急性心肌梗塞组血清MMP-2水平明显高于不稳定性心绞痛组;急性心肌梗塞组及不稳定性心绞痛组血清MMP-2水平明显高于正常对照组;稳定性心绞痛组与正常对照组差异无显著意义;急性心肌梗塞组及不稳定性心绞痛组血清MMP-2水平高于稳定性心绞痛组。结论急性冠脉综合征患者血清MMP-2水平明显升高,其水平可能与冠状动脉斑块的稳定性相关。     

Intimin及其受体Tir在致病性大肠杆菌致细胞线粒体功能障碍中的作用

目的探讨致病性大肠杆菌(Enteropathogenic Escherichia coli,EPEC)外膜蛋白Intimin及其受体Tir在EPEC致HeLa细胞线粒体功能障碍中的作用。方法将EPEC外膜蛋白Intimin及其受体Tir删除株、相应质粒互补株或染色体互补株感染HeLa细胞,用线粒体膜电位(Mitochondria membrane potential,MMP)检测试剂JC-1染色细胞线粒体,通过多功能酶标仪检测MMP水平,Western blot检测Intimin的表达及Tir的转位。结果与野生型菌株相比,Eae删除株和Tir删除株感染细胞的MMP功能显著减弱(P<0.05),Eae删除株功能能被质粒表达相应蛋白所互补,Tir删除株不能被质粒表达Tir互补,但可被染色质表达野生型Tir或TirY474S互补,而染色质TirS434A突变株不能引起明显的MMP下降。结论 Intimin和Tir是参与线粒体功能障碍的重要分子;TirS434在线粒体功能障碍中起重要作用。     

Mechanical Properties of Melt-processed Blend of Amorphous Corn Flour Composite Filler and Styrene-Butadiene Rubber

The corn flour composite fillers were prepared by blending corn flour with rubber latex, dried, and cryogenically ground into powders, which were then melt-blended with rubber polymers in an internal mixer to form composites with enhanced mechanical properties. The composites prepared with melt-blending method were compared to those prepared with a freeze-drying method. The composite fillers prepared with styrene-butadiene were compared to those made with carboxylated styrene-butadiene matrix. Dynamic effects showed that the corn flour composite fillers produced composites with good tensile strength, elongation ratio, and toughness at 500 mm/min strain rate. Tear resistance of different composites was also studied.     

Polyamide 66 nanocomposites based on organoclays treated with thermally stable phosphonium salts

Purification of bentonite clays and their modification with two thermally stable (alkyl and aryl) phosphonium organic salts were investigated. The organoclays were subsequently melt compounded with Polyamide 66 (PA66), with and without the use of an elastomeric compatibilizer. The morphology, melt flow, thermal stability, and mechanical properties of the binary and ternary nanocomposites were studied. The bentonite clay was purified by sedimentation, resulting in higher cation exchange capacity and thermal stability in comparison with unpurified clay. These were then used in the synthesis of two thermally stable organoclays by replacing the interlayer sodium cations with two (alkyl and aryl) phosphonium surfactant cations to circumvent the problem of low temperature decomposition of quaternary ammonium organoclays usually used in polymer nanocomposites. The organoclay with aliphatic groups showed more compatibility with PA66 in comparison with the organoclay with aromatic groups. Thus, the use of organoclay with aliphatic groups resulted in nanocomposites with higher tensile strength, higher modulus, higher elongation at break, and higher impact strength in comparison with the nanocomposites produced from the organoclay with aromatic groups. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

三七叶甙制备原人参二醇及其差向异构体

三七叶总甙以c(NaOH)=2mol/L的氢氧化钠水溶液溶解,沸水浴加热8h进行水解,所得产物经乙酸乙酯萃取和硅胶柱层析分离得到原人参二醇。三七叶总甙与浓盐酸常温反应7h后,再用饱和碳酸钠溶液常温搅拌24h,所得产物经乙酸乙酯萃取和硅胶柱层析分离得到20(R) 原人参二醇。它们的结构经光谱分析及与文献对照得以鉴定。     

Electromechanical behavior of hybrid carbon/glass fiber composites with tension and bending

To understand the smart (i.e., good memory) characteristics of hybrid composites of carbon fibers (CFs) and glass fibers (GFs) with epoxy resin as a matrix, the changes in the electrical resistance of composites with tension and on bending were investigated. The electrical resistance behavior of composites under tension changed with the composition of the CF/GF, as well as with the applied strain. The fractional electrical resistance increased slowly with increasing strain within a relatively low strain region. However, with further loading it increased stepwise with the strain according to the fracture of the CF layers. The strain sensitivity of the samples increased with increasing CF weight percentage, and the samples incorporating more than 40 wt % CF showed a strain sensitivity higher than 1.54 for a single CF. The changes in the fractional electrical resistance with bending were not so dominant as those with tension. This difference was attributed to the action of two cancelling effects, which are the increasing and decreasing fractional electrical resistance due to tension and compression with bending, respectively. On recovery from a large applied bending, the fractional electrical resistance decreased slowly with unloading because of the increase of contacts between the fibers that resulted from the reorganization of ruptured CFs during the recovery. Even the composites incorporating a relatively small CF content showed an irreversible electrical resistance with both tension and bending. However, the strain sensitivity being larger with tension than with bending is ascribed to the difference in their mechanical behaviors. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2447–2453, 2002     

Specific determination of malonaldehyde by N-methyl-2-phenylindole or thiobarbituric acid

Reactivity of a commercially available test kit (LPO-586), based on N-methyl-2-phenylindole, toward aldehydes was characterized and compared with that of thiobarbituric acid (TBA). In hydrochloric acid, LPO-586 produced a violet pigment with malonaldehyde (MA) but not with other tested aldehydes. In methane sulfonic acid, LPO-586 produced the violet pigment with MA and 4-hydroxynonenal (HNE), but not with other tested aldehydes. Pigment formation with MA was not inhibited by other aldehydes, but that with HNE was inhibited by alka-2,4-dienals. TBA produced a red pigment with MA but not with other tested aldehydes in hydrochloric acid or in acetate with ethylenediaminetetraacetic acid (EDTA). Both the LPO-586 test in hydrochloric acid and the TBA test in hydrochloric acid or in acetate with EDTA can be used for specific measurement of MA in oxidized lipid samples.