苯并噻唑盐催化多聚甲醛合成1,3-二羟基丙酮

在氮气保护下,以多聚甲醛为原料,正丁醇作溶剂,三乙胺作助催化剂,在溴化-3-乙基苯并噻唑盐催化作用下合成了1,3-二羟基丙酮。考察了反应温度、反应时间、三乙胺用量对产物1,3-二羟基丙酮(DHA)收率的影响,得出的优选工艺参数为:60 mmol多聚甲醛,3 mmol催化剂和25 mL三乙胺,同时加入10 mL正丁醇,反应温度130℃,反应时间40 min。DHA收率为37%,选择性在95%～98%。产物经过先酯化再水解分离的提纯工艺,质量分数从90%提高到99.8%,分离提纯后得率为72%。产物熔点为73℃;通过IR、1HNMR及紫外可见光谱分析确证了化合物的结构。     

花片状钌纳米颗粒的控制合成

以三氯化钌为前驱体、聚乙烯吡咯烷酮（PVP）为稳定荆、三缩四乙二醇（TEG）和Zn粉为还原剂,于170℃反应2h。再加入适量十六烷基三甲基溴化铵（CTAB）,继续反应4h成功制得花片状Ru纳米颗粒。反应体系中最适宜RuCl2：PVP：CTAB：Zn（摩尔比）为1：20：1：1．5。产物用透射电子显微镜（TEM）、X-射线粉末衍射（XRD）、紫外可见吸收光谱（UV—Vis）等进行了表征。     

白藜芦醇关键中间体的合成工艺研究

改进了合成白藜芦醇的关键中间体3,5-二羟基-4’-甲氧基-1,2-二苯乙烯(1.3)的合成工艺。3,5-二乙酰氧基苄基三苯基膦溴化盐(1)与茴香醛在DMF中以CH3ONa为碱会发生Wittig反应,当1与CH3ONa的摩尔比为1:1时,反应的主产物有3个,分别为3,5-二乙酰氧基-4’-甲氧基-1,2-二苯乙烯(1.1)、3-乙酰氧基-5-羟基-4’-甲氧基-1,2-二苯乙烯(1.2)和3,5-二羟基-4’-甲氧基-1,2-二苯乙烯(1.3);当1与CH3ONa的摩尔比在1:2~3时,反应主产物是1.3。3,5-二羟基苄基三苯基膦溴化盐(2)与茴香醛在DMF中以CH3ONa为碱也会发生同样的反应,且当2与CH3ONa的摩尔比为1:1时,主产物是1.3。当1与CH3ONa的摩尔比为1:5时,没有Wittig反应产物生成。因此,按上述反应条件制得1.3后再去掉其上的甲基保护基团即可得白藜芦醇,相比其他的合成白藜芦醇工艺,省去了去乙酰基团的反应步骤。     

CTAB存在下纳米Pd粒子的超声诱导生长

在微量十六烷基三甲基溴化铵(CTAB)存在下,超声辐射PdCl2的乙醇水溶液,制得了纳米Pd粒子,用XRD、UV、TEM和HRTEM等进行了表征,探讨了超声诱导纳米Pd粒子的生长过程。结果表明,当超声辐射50min时,得到呈多边形的纳米Pd粒子,粒径分布较集中,大约为10nm。     

超声波辐射及相转移催化合成大茴香腈

以大茴香醛为原料,采用超声波辐射和相转移催化法直接合成大茴香腈的最佳反应条件为:n(大茴香醛)∶n(盐酸羟胺)=1∶(1.4～1.6),反应温度80℃,超声波辐射功率200W,辐射时间60min。在该条件下,相转移催化剂CTMAB的用量m(CTMAB)/m(大茴香醛)=0.06时,大茴香腈产率可达90.9%。     

Hydrate-based pre-combustion carbon dioxide capture process in the system with tetra-n-butyl ammonium bromide solution in the presence of cyclopentane

Effects of 0.29 mol% tetra-n-butyl ammonium bromide (TBAB) solution in conjunction with cyclopentane (CP) on the hydrate-based pre-combustion CO₂ capture are investigated by the measurements of the gas uptakes, CO₂ separation efficiencies and induction time of the hydrate formation at the different temperature-pressure conditions. The results show that the volume of the TBAB has an effect on the CO₂ separation and the induction time, and the addition of the CP into the TBAB solution remarkably enhances the CO₂ separation and shortens the induction time. The system with the CP/TBAB solution volume ratio of 5 vol% and TBAB solution/reactor effective volume ratio of 0.54 is optimum to obtain the largest gas uptake and the highest CO₂ separation efficiency at 274.65 K and 4.0 MPa. Compared to the results with tetrahydrofuran (THF) as an additive [1], the gas uptake is enhanced by at least 2 times and the induction time is shortened at least 10 times at the similar temperature-pressure condition. In addition, the CO₂ concentration in the decomposed gas from the hydrate slurry phase reaches approximately 93 mol% after the first-stage separation at 274.65 K and 2.5 MPa. The gas uptakes of more than 80 mol% are obtained after 400 s at the temperature range of 274.65-277.65 K and the pressure range of 2.5-4.5 MPa.     

The interaction of sesamol with DNA and cytotoxicity,apoptosis, and localization in HepG2 cells

Sesamol, a nutritional antioxidant phenolic compound present in sesame seed, has a potential therapeutic molecule effect against cancers. In this study, the interaction between sesamol and DNA was investigated by employing ultraviolet/visible (UV/Vis), fluorescence, circular dichroism (CD), Fourier transform infrared spectroscopy (FT-IR), and molecular modeling. The fluorescence analysis indicated that the fluorescence quenching mechanism of sesamol by calf thymus DNA (ctDNA) occurred through static quenching. The UV/Vis, CD, FT-IR spectra and molecular docking results implied that the primary binding mode was minor groove binding. Furthermore, the intracellular interaction of sesamol with DNA and its bioactivity effect were explored. The cell activity results demonstrated that sesamol induced hepatic cell line (HepG2) death. The acridine orange (AO)/ethidium bromide (EB) staining assay and DNA fragmentation confirmed that sesamol could efficiently induce the apoptosis of HepG2 cells. Moreover, addition of sesamol to HepG2 cells resulted in nuclear localization, as visualized by confocal microscopy.     

四丁基溴化铵水合物储存氢气的研究

利用高压搅拌式水合物实验装置,进行了四丁基溴化铵(TBAB)水合物储氢的研究。在恒容条件下,考察了水浴温度、初始压力对水合物储氢特性的影响,并比较了TBAB水合物和四氢呋喃(THF)水合物的储氢性能。实验结果表明,在初始压力7.2 MPa、x(TBAB)=0.6%的条件下,水浴温度越低,生成水合物的诱导时间越短,储氢密度越大,水浴温度为0.5℃时储氢密度最大(为0.095%);在水浴温度0.5℃、x(TBAB)=0.6%的条件下,初始压力越大,生成水合物的诱导时间越短,储氢密度越大,在初始压力为8.4 MPa时储氢密度最大(为0.109%);在水浴温度为0.5℃、初始压力7.2 MPa的条件下,THF水合物的储氢密度仅为0.014%,远低于TBAB水合物的储氢密度(0.095%),TBAB水合物的储氢性能更好。     

十六烷基三甲基溴化铵和FC911对砂岩表面润湿性的影响

分别用十六烷基三甲基溴化铵（CTAB）和阳离子氟碳型表面活性剂FC911处理石英砂,然后用Washburn法测定处理后石英砂对水和油的接触角,研究两种阳离子表面活性剂对砂岩表面润湿性的影响。实验结果表明随着处理液CTAB浓度从0增至10000 mg/L,石英砂水相接触角由0°增至89°,再减至66°,表面从水湿变为中性润湿,再变为弱水湿。FC911浓度为10～1000 mg/L时,水相接触角由〉90°逐渐减小至89.7°;油相接触角由15.3°逐渐增至〉90°。石英砂表面由强油湿变为弱油湿后再变为中间气湿。较低浓度的FC911即可将石英砂表面转变为既疏水又疏油的中间气湿,最佳使用浓度为200 mg/L。     

粉唑醇的合成

粉唑醇是用于植物叶片和穗的广谱杀菌剂,对谷物白粉病、云形病、叶斑病和锈病都有效。本文以邻氟溴苯为原料经格氏反应合成1-(2-氟苯基)-1-(4-氟苯基)-2-氯乙醇,然后与1,2,4-三唑钠盐反应得到标题化合物。总收率达59%,含量94.5%。